HRID1486653

反应详情

EQUATION

反应方程式

HRID 1486653 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

A mixture of 1-(6-bromopyridin-3-yl)ethanone (200 mg, 1.0 mmol) and CuCN (179 mg, 2.0 mmol) in anhydrous DMF (5 mL) was heated at 110° C. for 18 h under N2. The mixture was cooled to room temperature and diluted with water. After addition of EtOAc and filtration, the aqueous layer was extracted with EtOAc. The organic layer was washed with sat. NaHCO3 (aq), brine, and then dried (MgSO4) and concentrated. The product 5-acetylpicolinonitrile (120 mg) was obtained by silica gel chromatography (elution with 0-20% EtOAc/Hex).

WORKUP

后处理

  1. temperatureThe mixture was cooled to room temperature
  2. extractionthe aqueous layer was extracted with EtOAc
  3. washThe organic layer was washed with sat. NaHCO3 (aq), brine
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated