HRID561412

反应详情

EQUATION

反应方程式

HRID 561412 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 2 h
  3. extractiontwo extractions with diethyl ether
  4. dry with materialthe combined organic phases were dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated