HRID381312

反应详情

EQUATION

反应方程式

HRID 381312 的结构方程式

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

Cuprous cyanide (12.8 g, 143 mmol) was added to a stirred solution of 6-bromo-1-methylindole (10 g, 47 mmol) in N-methylpyrrolidinone (60 ml) under a nitrogen atmosphere. The reaction mixture was heated at 150° C. for 48 h. The reaction mixture was cooled and partitioned between ethyl acetate (200 ml) and aqueous ammonia (200 ml of 0.88 M). The organic layer was washed with brine (3×200 ml), dried (MgSO4) and concentrated. Flash column chromatography (elution with 70% hexane/30% ethyl acetate) gave the product as a crystalline white solid (5.3 g).

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled
  2. custompartitioned between ethyl acetate (200 ml) and aqueous ammonia (200 ml of 0.88 M)
  3. washThe organic layer was washed with brine (3×200 ml)
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated
  6. washFlash column chromatography (elution with 70% hexane/30% ethyl acetate)