HRID1051126

反应详情

EQUATION

反应方程式

HRID 1051126 的结构方程式

CONDITIONS

反应条件

温度
115 °C

PROCEDURE

实验过程

A mixture of 5-nitro-3-(trifluoromethyl)pyridin-2(1H)-one 3 (1.50 g, 7.21 mmol), POCl3 (2.76 g, 18.02 mmol) and PCl5 (1.4 g, 10.09 mmol) is heated to about 110-120° C. for 8 hours and then poured into ice water. The mixture is neutralized with solid NaHCO3 and extracted with ethyl acetate (3×40 ml). The combined organic phases is dried over Na2SO4 and all solvents removed under reduced pressure to obtain 2-chloro-5-nitro-3-(trifluoromethyl)pyridine 4.

WORKUP

后处理

  1. extractionextracted with ethyl acetate (3×40 ml)
  2. dry with materialThe combined organic phases is dried over Na2SO4
  3. customall solvents removed under reduced pressure