HRID1008754

反应详情

EQUATION

反应方程式

HRID 1008754 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

Lithium sulfide (3.5 g) (supplied from Aldrich) was added to a solution of 10.1 g of 2,5-difluorobenzophenone in 200 mL of DMSO, and stirred at 120° C. under a nitrogen atmosphere for 3 hours. Under ice cooling, 200 mL of 1 N hydrochloric acid was added to the reaction solution. Further 400 mL of ethyl acetate and 200 mL of water were added thereto, and the mixture was separated into two liquid phases. The organic layer was washed with 400 mL of water, and then washed with 200 mL of saturated brine. The organic layer was dried on sodium sulfate anhydrate and subsequently concentrated, to yield 10.54 g of the title compound.

WORKUP

后处理

  1. customthe mixture was separated into two liquid phases
  2. washThe organic layer was washed with 400 mL of water
  3. washwashed with 200 mL of saturated brine
  4. customThe organic layer was dried on sodium sulfate anhydrate
  5. concentrationsubsequently concentrated