HRID225766

反应详情

EQUATION

反应方程式

HRID 225766 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

N,N′-Carbonyldiimidazole (1 g, 6.17 mmol) was added to a solution of 6-bromonicotinic acid (1 g, 4.95 mmol) in dimethylsulfoxide (4.16 mL) and the mixture was stirred for 24 hours. Dimethylamine (40% in water, 8.3 mL, 37 mmol) was then added and the mixture was stirred for a further 18 hours. The reaction mixture was then diluted with dichloromethane (20 mL) and washed with water (10 mL). The organic layer was dried over sodium sulphate and concentrated in vacuo. The residue was purified by column chromatography on silica gel, eluting with ethyl acetate to afford the title compound in 46% yield, 520 mg.

WORKUP

后处理

  1. stirringthe mixture was stirred for a further 18 hours
  2. washwashed with water (10 mL)
  3. dry with materialThe organic layer was dried over sodium sulphate
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by column chromatography on silica gel
  6. washeluting with ethyl acetate