HRID381312
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- temperatureThe reaction mixture was cooled
- custompartitioned between ethyl acetate (200 ml) and aqueous ammonia (200 ml of 0.88 M)
- washThe organic layer was washed with brine (3×200 ml)
- dry with materialdried (MgSO4)
- concentrationconcentrated
- washFlash column chromatography (elution with 70% hexane/30% ethyl acetate)