HRID127589

反应详情

EQUATION

反应方程式

HRID 127589 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To the solution of 4.0 g of phenylcarbamoyl-acetonitrile in 50 ml of dimethylformamide 28 g of potassium tert. butoxide are added while stirring under nitrogen. After 2 hours the resulting suspension is cooled to 5° and 4.0 g of 1-methylpyrrol-2-carboxylic acid chloride (U.S. Pat. No. 3,551,571) are added during 10 minutes. The mixture is stirred for 18 hours at room temperature, poured into 300 ml of ice water and the precipitate formed filtered off. It is washed with water, dried and recrystallized from ethanol, to yield the 1-methyl-β-oxo-α-phenylcarbamoyl-2-pyrrolpropionitrile melting at 172°-174°; it is identical with that obtained according to Example 1.

WORKUP

后处理

  1. temperatureAfter 2 hours the resulting suspension is cooled to 5°
  2. addition3,551,571) are added during 10 minutes
  3. stirringThe mixture is stirred for 18 hours at room temperature
  4. customthe precipitate formed
  5. filtrationfiltered off
  6. washIt is washed with water
  7. customdried
  8. customrecrystallized from ethanol