反応 #215126

反応方程式

HCl

Diphenylphosphoryl chloride

HCl

6-Aminonicotinamide

pyridine

→

6-diphenylphosphorylamino nicotinamide

溶媒

ethanol

Chloroform

2-pyrrolidinone

反応条件

後処理

1. 1
   その他After 1 hour of reaction at room temperature
2. 2
   その他A reddish syrup, 2.2 g which is formed in the bottom of the flask
3. 3
   その他is isolated by decantation
4. 4
   その他The product may be purified
5. 5
   その他The reddish syrup obtained
6. 6
   抽出to extract the product
7. 7
   乾燥After dried over anhydrous sodium sulfate the chloroform solution which
8. 8
   その他is evaporated at 35° C. in vacuum

実験手順

6-Aminonicotinamide 1.37 g (0.01 mole) is dissolved in 10 ml of 2-pyrrolidinone and 3 ml of pyridine by gentle warming of the mixture. Diphenylphosphoryl chloride 6 ml (0.024 mole) is then slowly added to the mixture. After 1 hour of reaction at room temperature, the mixture is poured into 300 ml of 0.2 N HCl. A reddish syrup, 2.2 g which is formed in the bottom of the flask is isolated by decantation. The product may be purified as follows. The reddish syrup obtained above is dissolved in 3 ml of ethanol and the solution is admixed with 200 ml of 0.2 N HCl. Chloroform, 100 ml is added to the mixture to extract the product. After dried over anhydrous sodium sulfate the chloroform solution which contains the product is evaporated at 35° C. in vacuum to give a practically pure 6-diphenylphosphorylamino nicotinamide.

出典