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Home made nembutal
Equipment
-hotplate
-stainless steel cup
-small cooking pot
-thermometer
-clamp-stand
-filter
-stainless steel stir rod
Reagents
-26.7 g of clean metallic sodium
-400 g of anhydrous (dry) Ethanol
-32.7g of Urea, molecular biology grade, CH4N2O, FW=60 g/mol
-Solution of 100 g of 1-methyl butyl-ethyl malonic ester(Propanedioic acid)
-Water
PROCEDURE
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.
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.
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.
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.
5) Another 10.9 g of urea is added and allowed to react for 35 minutes.
6) The last 10.9 g of urea is added and allowed to react for 30 minutes.
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 .
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 .
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