HRID127584

反应详情

EQUATION

反应方程式

HRID 127584 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To the suspension of 12.9 of 1-methyl-β-oxo-2-pyrrolpropionitrile in 150 ml of dry toluene and 10.1 g of anhydrous triethylamine, 10.7 g of phenylisocyanate are added while stirring. After all solids are dissolved, the dark red solution is allowed to stand 30 minutes at room temperature, 5 minutes on the steam cone and at room temperature overnight. The mixture is evaporated on the steam cone, the residue taken up in methanol and the solution poured into the mixture of 25 ml of 5 N hydrochloric acid and 600 ml of water. The light brown crystals formed are collected, washed with water, triturated with ethanol and recrystallized from about 2200 ml of methanol, to yield the 1-methyl-β-oxo-α-phenylcarbamoyl-2-pyrrol-propionitrile of the formula ##STR8## melting at 174°-175°.

WORKUP

后处理

  1. additionare added
  2. dissolutionAfter all solids are dissolved
  3. customThe mixture is evaporated on the steam cone
  4. additionthe solution poured into the mixture of 25 ml of 5 N hydrochloric acid and 600 ml of water
  5. customThe light brown crystals formed
  6. customare collected
  7. washwashed with water
  8. customtriturated with ethanol
  9. customrecrystallized from about 2200 ml of methanol