HRID910699

反应详情

EQUATION

反应方程式

HRID 910699 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A mixture of 3-(4-chloro-pyridin-2-yl)-thiophene-2-carbaldehyde (103 mg, 0.46 mmol) and hydroxylamine hydrochloride (70 mg, 1 mmol) in pyridine (1 mL) was heated at 80° C. for 30 minutes. Acetic anhydride (0.8 mL) was added and the resulting mixture was heated at the temperature for another 3 hours. Ice water was added, the water solution was extracted with EtOAc and organic layer was concentrated. The resulting residue was purified by silica gel column to yield 3-(4-chloro-pyridin-2-yl)-thiophene-2-carbonitrile.

WORKUP

后处理

  1. temperaturethe resulting mixture was heated at the temperature for another 3 hours
  2. extractionthe water solution was extracted with EtOAc and organic layer
  3. concentrationwas concentrated
  4. customThe resulting residue was purified by silica gel column