HRID1042138

反应详情

EQUATION

反应方程式

HRID 1042138 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A mixture of 4-fluoro-2-methyl-1-nitrobenzene (9.4 g), 6-(methylsulfonyl)pyridin-3-ol (10.0 g), potassium carbonate (8.8 g), and N,N-dimethylformamide (100 mL) was stirred at 60° C. for 24 hr. The reaction solution was concentrated under reduced pressure, and the obtained residue was added to a mixture of ethyl acetate-water. The precipitated solid was collected by filtration, washed with water and ethyl acetate and dried to give the title compound (8.28 g) as a pale-yellow solid. The filtrate was extracted with ethyl acetate, washed successively with aqueous citric acid solution, water and brine, dried over magnesium sulfate, filtered and concentrated under reduced pressure. The obtained solid was washed with ethyl acetate to give the title compound (4.30 g) as a pale-yellow solid.

WORKUP

后处理

  1. concentrationThe reaction solution was concentrated under reduced pressure
  2. additionthe obtained residue was added to a mixture of ethyl acetate-water
  3. filtrationThe precipitated solid was collected by filtration
  4. washwashed with water and ethyl acetate
  5. customdried