HRID561412
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
PROCEDURE
实验过程
3.5 ml (3.50 mmol) of a 1N solution of chlorophenylmagnesium bromide in diethyl ether were introduced into 5 ml of THF at RT under argon, a solution of 490 mg (3.18 mmol) of the compound from Example 73A in 5 ml of tetrahydrofuran was added, and the mixture was heated under reflux for 2 h. Saturated aqueous ammonium chloride solution was added, two extractions with diethyl ether were carried out, and the combined organic phases were dried over sodium sulfate, filtered and concentrated. 714 mg of the title compound with a purity of 54% (59% of theory) were obtained and were reacted without further purification.
WORKUP
后处理
- temperaturethe mixture was heated
- temperatureunder reflux for 2 h
- extractiontwo extractions with diethyl ether
- dry with materialthe combined organic phases were dried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated