TheDeanVanGreunen

LSD Bro ;)

Feb 9th, 2018
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  1. How to make LSD
  2.  
  3.  
  4.  
  5. [All text used without permission
  6. from the "Whole Drug Manufacturers Catalog"
  7. Any typos are YOUR problem
  8. For informational purposes only
  9. I take NO responsibility for YOUR actions
  10. Be careful --Ed.]
  11.  
  12.  
  13.  
  14. NOTE: the techniques described herein are potentially dangerous. It
  15. is highly recommended that the physical and chemical properties of
  16. the reagents used and the reactions employed be given further study
  17. by persons unfamiliar with them. For the layman to attempt these
  18. procedures without first thoroughly preparing himself is to invite
  19. almost certain disaster. The publishers therefore disclaim
  20. responsibility for any damage or injury resulting from the improper
  21. handling of the chemicals and techniques described, and strongly
  22. urge all persons unqualified to perform the reactions to use
  23. extraction rather than synthesis.
  24.  
  25.  
  26.  
  27. #1: Kitchen chemistry
  28.  
  29. Extraction of LSA (Lysergic acid amide)
  30. from Morning Glory (Ipomosea Purpurea) seeds
  31. or Hawaiian Baby Wood Rose (Argyreia Nervosa) seeds
  32.  
  33.  
  34. NOTE: Morning Glory seeds may be coated with a toxic chemical by
  35. the seed company in order to prevent ingestion. If a packet of
  36. seeds contains coated seeds this fact should be stated on the
  37. container. Soaking the seeds in warm water for 1/2 hour and
  38. rinsing in a strainer should remove this coating.
  39.  
  40. NOTE: while many varieties of morning glory contain the active LSA
  41. (Lysergic acid amide), the yield varies greatly. Therefore, use
  42. only Pearly Gates, Wedding Bells, and Heavenly Blue varieties for
  43. best results.
  44.  
  45.  
  46. Kitchen chemistry follows.
  47.  
  48.  
  49. Materials: blender, funnel, filter paper, petroleum ether or
  50. lighter fluid, methanol (wood alcohol), glass jar,
  51. Pyrex baking dish
  52.  
  53.  
  54. Grind Morning Glory or Hawaiian Baby Wood Rose seeds in a
  55. blender until they are a fine powder, and spread them out to
  56. dry.
  57. Soak the powder with lighter fluid or petroleum ether. Cap
  58. the container to avoid fumes, and don't smoke nearby, or
  59. you'll be very sorry.
  60.  
  61. In a well-ventilated area (neither ether nor lighter fluid are
  62. good for you), filter the solution through filter paper in a
  63. funnel. Discard the filtrate (the liquid).
  64.  
  65. Dry mash completely.
  66.  
  67. Soak mash in methanol (wood alcohol) for 2 days. Be careful
  68. -
  69. its vapors are poisonous and may be explosive.
  70.  
  71. Filter, and save the filtrate.
  72.  
  73. Soak the mash in methanol again a further 2 days.
  74.  
  75. Filter. Discard the mash, save the filtrate.
  76.  
  77. Pour both filtrates into a large, flat dish and evaporate in
  78. the absence of direct sunlight. Sunlight will break down the
  79. LSA. Preferably, perform ALL procedures in a cool, well-
  80. ventilated place away from sunlight.
  81.  
  82. After evaporation, a yellow gum will remain in the dish.
  83. Scrape it up.
  84.  
  85. To dose on the LSA, add some harmless filler (starch, flour,
  86. milk sugar) to the gum until it is not sticky. Put in gelatin
  87. capsules or take as is. 30 g Morning Glory seeds or 15
  88. Hawaiian Baby Woodrose seeds should make a goodly trip, so
  89. adjust dosage accordingly.
  90.  
  91. If you want to turn LSA into LSD, you can [see below], but
  92. it's MUCH more difficult and VERY unsafe.
  93.  
  94.  
  95.  
  96.  
  97. #2: Extraction of Lysergic Acid Amides
  98.  
  99.  
  100. Start with domestic Morning Glory seeds, the young seeds of
  101. the Hawaiian Baby Wood Rose, cultured ergot or naturally
  102. occurring ergot compounds.
  103.  
  104.  
  105. NOTE: Morning Glory seeds may be coated with a toxic chemical by
  106. the seed company in order to prevent ingestion. If a packet of
  107. seeds contains coated seeds this fact should be stated on the
  108. container. Soaking the seeds in warm water for 1/2 hour and
  109. rinsing in a strainer should remove this coating.
  110.  
  111. NOTE: while many varieties of morning glory contain the active LSA
  112. (Lysergic acid amide), the yield varies greatly. Therefore, use
  113. only Pearly Gates, Wedding Bells, and Heavenly Blue varieties for
  114. best results.
  115.  
  116.  
  117. Reduce seed material to a fine powder in a blender, and spread
  118. it out to dry. Grind again if not fine enough after the first
  119. time due to dampness.
  120.  
  121. Saturate powdered seed material with lighter fluid, naphtha or
  122. ligroine. When completely saturated, it should have the
  123. consistency of soup.
  124.  
  125. Pour into a chromatography column and let it sit overnight.
  126.  
  127. Remove the fatty oils from the material by dripping the
  128. solvent through the column slowly, and testing the liquid that
  129. comes through for fats by evaporating a drop on clean glass
  130. until it leaves no greasy film. (It should take several
  131. ounces of solvent for each ounce of seeds).
  132.  
  133. Mix 9 volumes of chloroform with 1 volume of concentrated
  134. ammonium hydroxide and shake in a separatory funnel. When it
  135. settles, the chloroform layer will be on the bottom. Drain
  136. the chloroform layer and discard the top layer.
  137.  
  138. Drip the chloroform wash through the column and save the
  139. extract. test continuously by evaporating a drop on clean
  140. glass until it ceases to fluoresce.
  141.  
  142. [It is NOT explicit in the source, but if extracting
  143. from ergot, I would start with the ergot alkaloid base at
  144. this point. --Ed.]
  145.  
  146. Evaporate the chloroform extracts, and dissolve the residue in
  147. the minimum amount of a 3% tartaric acid solution. If all the
  148. residue doesn't dissolve, place it into suspension by shaking
  149. vigorously.
  150.  
  151. Color the solution with an acid base indicator, and titrate to
  152. find the approximate number of moles of the alkaloid present.
  153.  
  154. Transfer the solution to a separatory funnel, and wash the
  155. other vessel with acid in order to get all the alkaloid out.
  156. Pour the washings in the funnel also.
  157.  
  158. Bring the pH up to make the solution basic by adding sodium
  159. bicarbonate solution, and add an equal volume of chloroform.
  160.  
  161. Shake thoroughly, let it settle, remove the bottom layer and
  162. set aside.
  163. Again add an equal portion of chloroform, shake, let settle
  164. and remove bottom layer.
  165.  
  166. Combine chloroform extracts (bottom layers) and evaporate.
  167.  
  168. The residue remaining after evaporation is a semi-pure
  169. concentrate of LSA (lysergic acid amide). The amide requires
  170. some experimentation for dosage, but 1 mg of the concentrate
  171. is a reasonable starting point. 1 mg LSA will produce effects
  172. comparable to 100 micrograms of LSD.
  173.  
  174.  
  175.  
  176.  
  177. #3: Ergot culture
  178.  
  179.  
  180. NOTE: contact with ergot compounds can be dangerous. Only after a
  181. basic understanding of the techniques employed in the handling of
  182. dangerous or poisonous organisms is reached should one proceed with
  183. the culture of ergot.
  184.  
  185. The need for absolute sterility cannot be overstressed. Consult
  186. any elementary text on bacteriology for the correct equipment and
  187. procedures. Avoid prolonged contact with ergot compounds, as they
  188. are poisonous and can be fatal.
  189.  
  190.  
  191. A) Get a source for Claviceps Purpurea fungus
  192.  
  193.  
  194. If no source can be found, you can make a field trip to obtain
  195. it from rye or other cereal grasses. Rye grass is the best
  196. choice. The ergot will appear as a blackish growth on the
  197. tops of the rye where the seeds are. They are approximately
  198. the same shape as the seeds and are referred to as "heads" or
  199. "ergot". From these heads or ergot sprout the Claviceps
  200. Purpurea fungi.
  201.  
  202. They have long stems and bulbous heads when viewed under a
  203. strong glass or microscope. It is these that must be removed
  204. from the ergot, free from contamination, and used to inoculate
  205. the culture material.
  206.  
  207.  
  208. B) Make a culture medium
  209.  
  210.  
  211. Combine the following ingredients in about 500 ml distilled
  212. water in a 2 L small-neck flask:
  213.  
  214.  
  215. Sucrose 100 g
  216.  
  217. Chick pea meal 50 g
  218. Calcium nitrate 1 g
  219. Ca(NO3)2
  220. Monopotassium phosphate 0.25 g
  221. KH2PO4
  222. Magnesium sulphate 0.25 g
  223. MgSO4
  224. Potassium chloride 0.125 g
  225. KCl
  226. Ferrous sulphate heptahydrate 8.34 mg
  227. FeSO47H20
  228. Zinc sulphate heptahydrate 3.44 mg
  229. ZnSO47H20
  230.  
  231.  
  232. Add water to make up one liter
  233.  
  234. Adjust to pH 4 with ammonia solution and citric acid
  235.  
  236. Sterilize by autoclaving
  237.  
  238.  
  239. C) Make a culture
  240.  
  241.  
  242. Inoculate the sterilized medium with Claviceps Purpurea under
  243. sterile conditions, stopper with sterilized cotton and
  244. incubate for two weeks, periodically testing and maintaining
  245. pH 4. After two weeks a surface culture can be seen on the
  246. medium. Large-scale production of the fungus can now begin.
  247.  
  248.  
  249. D) Large-scale production
  250.  
  251.  
  252. Obtain several ordinary 1 gallon jugs.
  253.  
  254. Place a two-hole stopper in the necks of the jugs.
  255.  
  256. Fit a short (6 inch) tube in one hole, leaving two inches
  257. above the stopper. Fit a short rubber tube to this. Fill a
  258. small (500 ml) Erlenmeyer flask with a dilute solution of
  259. sodium hypochlorite (NaClO). Extend a glass tube from the
  260. rubber so the end is immersed in the hypochlorite.
  261.  
  262. Fit a long glass tube in the other stopper hole. It must
  263. reach near the bottom of the jug and have about two inches
  264. showing above the stopper. Attach a rubber tube to the glass
  265. tube and fit a short glass tube to the end of the rubber tube.
  266.  
  267.  
  268. Fill a large glass tube (1" x 6") with sterile cotton and fit
  269. one-hole stoppers in the ends. Fit the small glass tube in
  270. the end of the rubber tube into one stopper of the large tube.
  271. Fit another small glass tube into the other stopper. A rubber
  272. tube is connected to this and attached to small air pump
  273. (obtained from a tropical fish store).
  274.  
  275. With this aeration equipment you can assure a supply of clean
  276. air to the Claviceps Purpurea fungus while maintaining a
  277. sterile environment inside the solution.
  278.  
  279. Dismantle the aerators. Place all the glass tubes, rubber
  280. tubes, stoppers and cotton in a paper bag, seal tightly with
  281. wire staples and sterilize in an autoclave.
  282.  
  283. Fill the 1-gallon jugs 2/3 to 3/4 full with the culture medium
  284. and autoclave.
  285.  
  286. While these things are being sterilized, homogenize in a
  287. blender the culture already obtained and use it to inoculate
  288. the material in the gallon jugs. The blender must be sterile.
  289.  
  290.  
  291. EVERYTHING must be sterile.
  292.  
  293.  
  294. Assemble the aerators. Start the pumps. A slow bubbling in
  295. each jug will provide enough oxygen to the cultures. A single
  296. pump may be connected to several filters.
  297.  
  298. Let everything sit at room temperature (25 C) in a dark place
  299. (never expose ergot alkaloids to bright light - they will
  300. decompose) for a period of ten days.
  301.  
  302. After ten days, adjust the culture to 1% ethanol using 95%
  303. ethanol under sterile conditions. Maintain growth for another
  304. two weeks.
  305.  
  306.  
  307. E) Extract ergot alkaloids
  308.  
  309.  
  310. After a total of 24 days growth period, the culture should be
  311. considered mature. Make the culture acidic with tartaric acid
  312. and homogenize in a blender for one hour.
  313.  
  314. Adjust to pH 9 with ammonium hydroxide and extract with
  315. benzene or chloroform/iso-butanol mixture.
  316.  
  317. Extract again with alcoholic tartaric acid and evaporate in a
  318. vacuum to dryness.
  319.  
  320. The dry material is the salt (the tartaric acid salt, the
  321. tartrate) of the ergot alkaloids, and is stored in this form
  322. because the free basic material is too unstable and decomposes
  323. readily in the presence of light, heat, moisture, and air.
  324.  
  325. To recover the free base for extraction of the amide or
  326. synthesis to LSD, make the tartrate basic with ammonia to pH
  327. 9, extract with chloroform, and evaporate in vacuo.
  328.  
  329.  
  330.  
  331.  
  332.  
  333. #4: Synthesis of LSD from ergot alkaloids or LSA
  334.  
  335. (including sections on isomerization, separation,
  336. purification & crystallization)
  337.  
  338.  
  339. NOTE: the chemicals and reactions described below are potentially
  340. dangerous even to an organic chemist in a well-equipped laboratory.
  341.  
  342. The publishers therefore disclaim responsibility for any damage or
  343. injury resulting from the improper handling of the chemicals and
  344. techniques described, and strongly urge all persons unqualified to
  345. perform the reactions to use instead the comparatively easier,
  346. safer ergot culture and LSA extraction process.
  347.  
  348.  
  349. A) Synthesis of LSD
  350. (iso- & dextro-lysergic acid diethylamide)
  351.  
  352.  
  353. PREPARATORY: obtain one red and one yellow photographic safety
  354. light and one weak, long-wave ultraviolet light. These are used to
  355. prevent the hydrolysis of lysergic acid compounds.
  356.  
  357. NOTE: Aluminum foil must be used to cover the chemicals when light
  358. is present. Rubber gloves must be worn; these compounds are
  359. extremely poisonous.
  360.  
  361. [The source implies but does not state that one may replace
  362. "ergot alkaloid" in the following with the seed-derived semi-
  363. pure LSA concentrate from #2. --Ed.]
  364.  
  365.  
  366. USING YELLOW LIGHT:
  367.  
  368. Place one volume of ergot alkaloid in a small roundbottom
  369. flask. Add 2 volumes of anhydrous hydrazine and reflux for 30
  370. minutes, or the mixture may be heated in a sealed tube at 112
  371. Celsius for 30 minutes. If the reflux technique is used,
  372. maintain atmospheric pressure by using an open container or
  373. fractionating column.
  374.  
  375. After heating/refluxing, add 1.5 volumes of water to the
  376. mixture and boil gently for 15 minutes. After boiling is
  377. complete, cool the mixture in a refrigerator until
  378. solidification. The solid material obtained is iso-lysergic
  379. acid hydrazide.
  380.  
  381. USING RED LIGHT:
  382.  
  383. Chill all chemicals (reagents) to be used to 0 Celsius. Place
  384. an open flask in an ice bath. Add 100 ml concentrated
  385. hydrochloric acid (chilled to 0 C).
  386.  
  387. Quickly add 2.82 g of the lysergic acid hydrazide to the
  388. hydrochloric acid, being careful to maintain a temperature of
  389. 0 Celsius.
  390.  
  391. Add 100 ml of a 0.1 N (1/10th Normal) solution of sodium
  392. nitrite (chilled to 0 C) and stir vigorously for 3 minutes.
  393.  
  394. Continue stirring at 0 Celsius and add dropwise 130 ml of the
  395. hydrochloric acid.
  396.  
  397. When the acid addition is complete, continue stirring for 5
  398. minutes, then neutralize the solution with sodium bicarbonate,
  399. using a saturated water solution of the bicarbonate.
  400.  
  401. Extract the solution with ether, remove the water layer, and
  402. dissolve the gummy substance in ether. Add this to the ether
  403. layer.
  404.  
  405. Add 3 g of diethylamine for every 30 ml of the ether extract.
  406.  
  407. Let this stand in the dark, and gradually warm up to 20
  408. Celsius for at least 24 hours.
  409.  
  410. Evaporate this solution in a vacuum.
  411.  
  412. The material remaining is a mixture of the inactive
  413. iso-lysergic acid diethylamide and the active lysergic acid
  414. diethylamide (LSD-25). The inactive isomer must now be
  415. converted (isomerized) to the active isomer to greatly
  416. increase the yield, since the inactive compound predominates
  417. in this synthesis.
  418.  
  419.  
  420.  
  421. B) Isomerization of iso-LSD into the active LSD-25
  422.  
  423.  
  424. USING THE RED LIGHT:
  425.  
  426. Dissolve the synthesized material into the minimum amount of
  427. ethyl alcohol.
  428.  
  429. Mix a 4 Normal solution of potassium hydroxide in ethanol.
  430. The amount of solution needed is twice the volume of the
  431. iso-LSD/ethanol solution.
  432.  
  433. Add the two solutions together and let the mixture sit for 4
  434. hours at room temperature.
  435.  
  436. Neutralize the mixture with dilute hydrochloric acid, then
  437. make it slightly basic with ammonium hydroxide.
  438.  
  439. Extract the mixture with chloroform, sparate the chloroform
  440. layer, and extract this four times with a 25% volume of water.
  441.  
  442. Evaporate the chloroform in a vacuum. Discard the water
  443. extracts. The material left after evaporation a mixture of
  444. iso-LSD and LSD-25, the active LSD predominating.
  445.  
  446. The mixture may now be separated by chromatography and the
  447. iso-LSD again isomerized by the above process.
  448.  
  449.  
  450.  
  451. C) Separation, purification & crystallization of LSD-25
  452.  
  453.  
  454. USING A DARKROOM:
  455.  
  456. The material obtained from the isomerization process is now
  457. dissolved in a solution prepared from 3 parts benzene/1 part
  458. chloroform. Use 50 ml solvent per 1 gram LSD material.
  459.  
  460. Mix a slurry basic alumina in benzene. Pack it into a 1 inch
  461. chromatoghraphy column until it fills 6 inches.
  462.  
  463. When the slurry settles, drain the benzene/chloroform down to
  464. the level of the basic alumina, and carefully add an equal
  465. amount of the LSD/solvent solution.
  466.  
  467.  
  468. USING A WEAK, LONG-WAVE ULTRAVIOLET LIGHT:
  469. (to follow the blue band only)
  470.  
  471. Drain the solution through the column. The fastest-moving,
  472. blue fluorescent band contains the LSD-25. Collect this
  473. fraction and evaporate in a vacuum. The syrup remaining will
  474. crystallize spontaneously, but slowly. Do not heat.
  475.  
  476. Use the UV light only whe necessary to follow the blue band in
  477. order to avoid decomposition of the compounds.
  478.  
  479. Dissolve the syrup or crystal in tartaric acid solution and
  480. recrystallize to form the stable end-product (dextro lysergic
  481. acid diethylamide tartrate).
  482.  
  483. The material remaining in the column may be removed with
  484. methanol, evaporated in a vacuum, and recycled through the
  485. isomerization and subsequent procedures by itself or combined
  486. with fresh material.
  487. Also, all leftover solutions and residues may be neutralized
  488. with socium bicarbonate, evaporated in vacuo, and extracted
  489. with ammoniacal chloroform, the extract evaporated to dryness,
  490. and the residue reused.
  491.  
  492.  
  493.  
  494.  
  495.  
  496. #5: Preparation of lysergic acid from the amide
  497.  
  498.  
  499. NOTE: this synthesis is as difficult and dangerous as the rest, and
  500. is of use only if using one of the following two LSD synthesis
  501. methods, which require lysergic acid as the starting compound. The
  502. lysergic acid amide obtained from the extract of ergot or seeds
  503. need not be converted to the acid prior to its use in the synthesis
  504. of LSD providing that the synthesis used is #4 given above, and
  505. giving the starting material "ergot alkaloid".
  506.  
  507.  
  508. Dissolve 10 g lysergic acid amide in 200 ml methanolic
  509. potassium hydroxide solution.
  510.  
  511. Remove the methanol by vacuum as soon as the amide is
  512. dissolved.
  513.  
  514. Dissolve the residue which is left into 200 ml of an 8%
  515. solution of potassium hydroxide in water.
  516.  
  517. Heat this mixture on a steam bath for 1 hour.
  518.  
  519. Pass a steam of nitrogen gas through the flask during the
  520. heating process. (The ammonia which is evolved in the gas
  521. stream may be titrated with hydrochloric acid in order to
  522. follow the reaction.)
  523.  
  524. Neutralize the mixture with tartaric acid (neutral to congo
  525. red) and run it through a filter paper.
  526.  
  527. Extract the mixture with ether in a separatory funnel. Save
  528. the water layer, discard the ether layer.
  529.  
  530. Filter the solution through a filter paper and evaporate.
  531.  
  532. Upon evaporation, dry crystals of lysergic acid will be
  533. obtained.
  534.  
  535.  
  536.  
  537.  
  538. #6: Synthesis of LSD
  539. using lysergic acid
  540. the quickest way to make pure LSD-25
  541. PREPARATORY: see #4
  542.  
  543. NOTE: The chemicals and techniques described are potentially
  544. dangerous. It is highly recommended that the physical and chemical
  545. properties of the reagents used be studied by those persons
  546. unfamiliar with them before the synthesis is attempted.
  547.  
  548.  
  549.  
  550. USING THE YELLOW LIGHT:
  551.  
  552. 5.36 g of d-lysergic acid are suspended in 125 ml
  553. acetonitrile, and the suspension is cooled to about -20
  554. Celsius in a bath of acetone cooled with dry ice.
  555.  
  556. To the suspension is added a cold (-20 C) solution of 8.82 g
  557. of trifluoracetic anhydride in 75 ml acetonitrile. The
  558. mixture is allowed to stand at -20 C for about 1 1/2 (one and
  559. one-half) hours.
  560.  
  561. (During this time the suspended material dissolves and the
  562. d-lysergic acid id converted to the mixed anhydride of
  563. lysergic and trifluoracetic acids.)
  564.  
  565. The mixed anhydride can be separated in the form of an oil by
  566. evaporating the solvent in vacuo at a temperature below about
  567. 0 Celsius.
  568.  
  569. Everything must be kept anhydrous.
  570.  
  571.  
  572. USING THE RED LIGHT:
  573.  
  574. The solution of mixed anhydrides in acetonitrile from above is
  575. added to 150 ml of acetonitrile containing 7.6 g of
  576. diethylamine.
  577.  
  578. The mixture is held in the dark at room temperature for about
  579. 2 hours.
  580.  
  581. The acetonitrile is evaporated in vacuo, leaving a residue of
  582. LSD-25 plus impurities.
  583.  
  584. The residue is dissolved in 150 ml of chloroform and 20 ml of
  585. ice water.
  586.  
  587. The chloroform layer is removed and the aqueous layer is
  588. extracted with several portions of chloroform. The chloroform
  589. portions are are combined and, in turn, washed with four 50 ml
  590. portions of ice-cold water.
  591.  
  592. The chloroform solution is then dried over anhydrous sodium
  593. sulfate and evaporated in vacuo.
  594.  
  595. NOTE: following the completion of this synthesis, follow the
  596. procedures described for separation, purification, and
  597. crystallization of LSD-25. If a higher yield is desired, follow
  598. the procedure on isomerization after doing the separation,
  599. purification, and crystallization.
  600.  
  601.  
  602.  
  603.  
  604. #7: Synthesis of LSD
  605. using lysergic acid
  606. high-yielding and fast
  607.  
  608.  
  609. PREPARATORY: see #4
  610.  
  611. NOTE: The chemicals and techniques described are potentially
  612. dangerous. It is highly recommended that the physical and chemical
  613. properties of the reagents used be studied by those persons
  614. unfamiliar with them before the synthesis is attempted.
  615.  
  616. NOTE: the following procedure gives good yield and is very fast,
  617. with little iso-lysergic acid being produced. However, the
  618. stoichiometry must be exact or yields will drop
  619.  
  620.  
  621. USING WHITE LIGHT:
  622.  
  623. Sulfur trioxide is produced in an anhydrous state by carefully
  624. decomposing anhydrous ferric sulfate at approximately 480
  625. Celsius. Store under anhydrous conditions.
  626.  
  627. USING WHITE LIGHT:
  628.  
  629. A carefully-dried 22 liter RB flask fitted with an ice bath,
  630. dropping funnel, and mechanical stirrer is charged with 10 to
  631. 11 liters of dimethylformamide (freshly distilled under
  632. reduced pressure).
  633.  
  634. The condenser and dropping funnel are both protected against
  635. atmospheric moisture.
  636.  
  637. 2 lb. of sulfur trioxide (Sulfan B) are introduced dropwise,
  638. very cautiously with stirring, during 4 to 5 hours. The
  639. temperature is kept at 0-5 Celsius throughout the addition.
  640.  
  641. After the addition is complete, the mixture is stirred for 1
  642. to 2 hours until some separated crystalline sulfur trioxide-
  643. dimethylformamide complex has dissolved.
  644.  
  645. The reagent is transferred to an air-tight automatic pipette
  646. for convenient dispensing, and kept in the cold. Although the
  647. reagent, which is colorless, may change to yellow and red, its
  648. efficiency remains unimpaired for three to four months in cold
  649. storage.
  650.  
  651. An aliquot is dissolved in water and titrated with standard
  652. NaOH to a phenolphthalein end point.
  653.  
  654.  
  655. USING RED LIGHT:
  656.  
  657. A solution of 7.15 g of d-lysergic acid monohydrate (25 mmol)
  658. and 1.06 g of lithium hydroxide hydrate (25 mmol) in 200 L of
  659. MeOH is prepared.
  660.  
  661. The solvent is distilled on the steam bath under reduced
  662. pressure.
  663.  
  664. The residue of glass-like lithium lysergate is dissolved in
  665. 400 ml of anhydrous dimethyl formamide.
  666.  
  667. From this solution, about 200 ml of the dimethyl formamide is
  668. distilled off at 15mm pressure through a 12-inch helices
  669. packed column.
  670.  
  671. The resulting anhydrous solution of lithium lysergate left
  672. behind is cooled to 0 Celsius and, with stirring, treated
  673. rapidly with 500 ml of SO3DMF solution (1.00 Molar).
  674.  
  675. The mixture is stirred in the cold for 10 minutes and then
  676. 9.14 g (125.0 mmol) of diethylamine is added.
  677.  
  678. The stirring and cooling are continued for 10 minutes longer,
  679. when 400 ml of water is added to decompose the reaction
  680. complex.
  681.  
  682. After mixing thoroughly, 200 ml of saturated aqueous saline
  683. solution is added. The amide product is isolated by repeated
  684. extraction with 500 ml portions of ethylene dichloride.
  685.  
  686. The combined extract is dried and then concentrated to a syrup
  687. under reduced pressure. Do not heat the syrup during
  688. concentration. The LSD may crystallize out, but the crystals
  689. and the mother liquor may be chromatographed according to the
  690. instructions in the synthesis of LSD #4.
  691.  
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  694.  
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  702.  
  703. "Raw Data for Raw Nerves"
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