HRID1592331

反应详情

EQUATION

反应方程式

HRID 1592331 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3-(4-fluorophenyl)-2,2-dimethylpropionic acid ethyl ester (10.0 g, 44.6 mmol, see Part 1 of Example 25a) and a solution of sodium hydroxide (25 g) in water (110 mL) was heated at reflux for 18 h and cooled to room temperature. The solution was stirred on an ice bath and acidified with concentrated aqueous hydrochloric acid. The resulting precipitate was collected by filtration, washed with water and dried under vacuum. The residue was stirred with dichloromethane and filtered, and the filtrate was concentrated to provide an off-white solid (7.60 g, 87%).

WORKUP

后处理

  1. temperatureat reflux for 18 h
  2. filtrationThe resulting precipitate was collected by filtration
  3. washwashed with water
  4. customdried under vacuum
  5. stirringThe residue was stirred with dichloromethane
  6. filtrationfiltered
  7. concentrationthe filtrate was concentrated