HRID887923

反应详情

EQUATION

反应方程式

HRID 887923 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Triethylamine (0.0106 mole) then acetyl chloride (0.0106 mole) were added to a solution of intermediate (21) (0.0032 mole) in DCM (40 ml) cooled in an ice bath under argon. The mixture was allowed to slowly warm to room temperature and stir overnight. The mixture was cooled in an ice bath and ice cold water (30 ml) was added. After stirring for 10 minutes, the mixture was filtered, and the solid was allowed to dry overnight. The residue was suspended in 50 ml water. The suspension was allowed to stir for 30 minutes, filtered, and dried overnight, yielding 0.40 g of 1-acetyl-2,3-dihydro-5-methoxy-1H-indole-2-carboxamide (intermediate 22, mp. 196-197° C.).

WORKUP

后处理

  1. temperaturecooled in an ice bath under argon
  2. temperatureThe mixture was cooled in an ice bath
  3. stirringAfter stirring for 10 minutes
  4. filtrationthe mixture was filtered
  5. customto dry overnight
  6. stirringto stir for 30 minutes
  7. filtrationfiltered
  8. customdried overnight