HRID1609275

反应详情

EQUATION

反应方程式

HRID 1609275 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

In 300 ml of N,N-dimethylformamide were suspended 30.8 g of thiosalicylic acid, 28.2 g of 2-fluoronitrobenzene and 69.0 g of potassium carbonate, and the mixture was stirred at 100° C. for 2 hours. After cooling, water was added and acidified with hydrochloric acid and the crystals separated out therefrom were collected by filtration and washed with water. The crystals were then dissolved in ethyl acetate and the solution was dried over magnesium sulfate and filtered. The filtrate was concentrated and the crystals separated out therefrom were collected by filtration and dried to give 42.6 g of the title compound as yellow prisms, m.p. 169°-171° C.

WORKUP

后处理

  1. temperatureAfter cooling
  2. customthe crystals separated out
  3. filtrationtherefrom were collected by filtration
  4. washwashed with water
  5. dissolutionThe crystals were then dissolved in ethyl acetate
  6. dry with materialthe solution was dried over magnesium sulfate
  7. filtrationfiltered
  8. concentrationThe filtrate was concentrated
  9. customthe crystals separated out
  10. filtrationtherefrom were collected by filtration
  11. customdried