HRID910699
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe resulting mixture was heated at the temperature for another 3 hours
- extractionthe water solution was extracted with EtOAc and organic layer
- concentrationwas concentrated
- customThe resulting residue was purified by silica gel column