HRID896519

反应详情

EQUATION

反应方程式

HRID 896519 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-dimethyl-propionic acid ethyl ester (10.0 g, 44.6 mmol) and a solution of sodium hydroxide (25 g) in water (110 mL) was heated to reflux for 18 hours. The resulting solution was cooled to room temperature, then was stirred on ice and acidified to about pH 1 with concentrated aqueous hydrochloric acid. The resulting precipitate was collected by filtration, washed thoroughly with water, and dried under vacuum. The solid was stirred in dichloromethane, and the mixture was filtered to remove a residual gelatinous solid. The filtrate was concentrated to provide a pale yellowish solid (7.60 g, 87%) which was used without further purification. 1H NMR (300 MHz, CDCl3) δ7.14 (m, 2H), 6.98 (t, J=8 Hz, 2H), 2.88 (s, 2H), 1.22 (s, 6H). Mass spec (ES−) m/z 195.2 (M−H−, 100%).

WORKUP

后处理

  1. temperatureto reflux for 18 hours
  2. filtrationThe resulting precipitate was collected by filtration
  3. washwashed thoroughly with water
  4. customdried under vacuum
  5. stirringThe solid was stirred in dichloromethane
  6. filtrationthe mixture was filtered
  7. customto remove a residual gelatinous solid
  8. concentrationThe filtrate was concentrated