Advertisement
Guest User

Untitled

a guest
May 24th, 2019
87
0
Never
Not a member of Pastebin yet? Sign Up, it unlocks many cool features!
text 5.36 KB | None | 0 0
  1. Pentobarbitone. (Called Nembutal or Pentobarbital.) 26.7 g of clean metallic sodium are dissolved in 400 g of anhydrous (dry) ethanol. To this, a solution of 100 g of 1-methyl butyl-ethyl malonic ester and 37.2 g of dry urea is added. The mixture is heated for 4 to 6 hours in an autoclave, or refluxed for 20 to 40 hours. The alcohol is then removed by distillation. The residue is dissolved in water and this aqueous solution is acidified with hydrochloric acid. The precipitated product is filtered, washed with cold water, and recrystallized from boiling water. Yield: depends on your ability to exclude H2O from the beginning of the reaction, mp: 127-130℃.
  2.  
  3. Synthesis of Malonic Acid
  4.  
  5. 100 g of powdered chloroacetic acid is treated with 150 g of broken ice and dissolved in 125 g of caustic soda (33 1/4%) solution. The solution should be made exactly neutral, if it is not already (this refers to the mixture). After neutralizing, add 69 g of 98% potassium cyanide in 130 g of water, which has been warmed to 40℃. An hour after the addition, the mixture is slowly warmed to 100℃ and held at this temp for an hour. Cool slowly to 25℃ and add another 125 g of 33 1/4% caustic soda solution. Slowly heat the mixture to 100℃ and hold at that temp until no more ammonia is evolved (2 to 3 hours). To test: add sodium hydroxide solution to a sample and boil. If no ammonia evolves, then the reaction is complete. When the reaction is complete, the solution is cooled, acidified with dilute HCl acid, and carefully evaporated to complete dryness on a water bath. The residue is powdered, extracted repeatedly with ether, and the ether is removed by gently heating on a water bath. You may purify further by dissolving in the minimum amount of caustic soda solution, boiling with decolorizing carbon, acidifying and extracting with ether, as before. Yield: 95 g, mp: 132℃.
  6.  
  7. Synthesis of Urea
  8.  
  9. 50 g of potassium cyanide is heated in an iron crucible under a large flame until it begins to fuse. 140 g of red lead is added in small portions, while the mixture is stirred with a rod. When the addition is complete and the frothing has stopped, the fused mass is poured onto an iron tray. When cold, the mass is separated from metallic lead, ground up, and digested with 200 cc of cold water for 1 hour. The filtrate from this mixture is treated with 25 g of ammonium sulphate and evaporated to dryness on a water bath. The residue is powdered well, transferred to a flask and is boiled with 3 installments of ethanol under reflux, to dissolve the urea from the potassium sulphate. Each of the 3 ethanol extracts is filtered, then combined, and evaporated to a small bulk, until crystals of urea separate on cooling and standing. Mp: 132℃.
  10.  
  11.  
  12. [추가자료]
  13.  
  14. How to make Nembutal Sodium
  15.  
  16. We at Peaceful Exit help people in need and we are very happy we have this part to play in people's lives.
  17. Below is a step by step guide on how to Make Nembutal :MATERIALS
  18.  
  19. Equipment
  20.  
  21. -hotplate
  22. -stainless steel cup
  23. -small cooking pot
  24. -thermometer
  25. -clamp-stand
  26. -filter
  27. -stainless steel stir rod
  28.  
  29. Reagents
  30.  
  31. -26.7 g of clean metallic sodium
  32. -400 g of anhydrous (dry) Ethanol
  33. -32.7g of Urea, molecular biology grade, CH4N2O, FW=60 g/mol
  34. -Solution of 100 g of 1-methyl butyl-ethyl malonic ester(Propanedioic acid)
  35. -Water
  36.  
  37. PROCEDURE
  38.  
  39.  
  40. 1) A hotplate was rested on the base of a clampstand. A cooking pot containing 400 g of anhydrous (dry) ethanol is placed on the hotplate stirrer and 26.7g of clean metallic sodium is dissolved in it.
  41.  
  42. 2) Into the stainless steel cup there is placed a Solution of 100 g of 1-methyl butyl-ethyl malonic ester(Propanedioic acid). The cup is then placed into the small cooking pot containing a mixture of the Ethanol and Sodium and secured with clamps to the clamp stand. The end of the thermometer is placed in the pot and positioned as close to the cup as possible.
  43.  
  44. 3) It is warmed to a temperature of 170°C for 10 minutes to remove any residual moisture. Throughout the reaction the temperature of the mixture is kept at 170°C and stirring is done frequently.
  45.  
  46. 4) 10.9 g of urea is added slowly, one scoop at a time and with good stirring. During this moisture (water) formed making the mixture damp. Over the course of 20 minutes the mixture gradually dries out and the amount of released gas lessens.
  47.  
  48. 5) Another 10.9 g of urea is added and allowed to react for 35 minutes.
  49.  
  50. 6) The last 10.9 g of urea is added and allowed to react for 30 minutes.
  51.  
  52. 7) After adding the total amount of urea over 1h 25 min, the mixture is dry, contained yellow and off-yellow-to-white granules, and still damp with the water and alcohol. The product is then heated at a temperature of 280°C directly on the hotplate for 1h 20mins. During this process the mixture is stirred every 15 minutes and off-yellow-to-white granules became more prominent and as yellow ones lessened. The precipitated product is washed with cold water , filtered and heated again for about 40 minutes at a temperature of 127-130°C until all the water is removed and the white powder(Nembutal Sodium) is formed .
  53.  
  54. 8) The Nembutal Sodium is allowed to cool and weighed. Yield is 23g. The product is 95-99% pure. You can also use a test kit to Check the purity .For all those searching for more information on how to make their own Nembutal or needs guidance during the process , contact us now: Email : peacefulexit@gmail.comWebsite: www.peacefulexit.tk
Advertisement
Add Comment
Please, Sign In to add comment
Advertisement