HRID899378

反应详情

EQUATION

反应方程式

HRID 899378 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

A mixture of 5.5 g (29.4 mmol) 2-chloro nicotinic acid ethyl ester, 4.0 g (29.4 mmol) 5-hydroxybenzofurazan and 20.1 g (61.7 mmol) cesium carbonate in 125 ml dry dimethylformamide was heated at 90° C. for five days. The mixture was poured into water and extracted with ethyl acetate. The ethyl acetate extracts were combined; washed successively with sodium bicarbonate solution, water, and brine; then dried (Na2SO4); and concentrated in vacuo to give a solid. Recrystallization from diethyl ether/pentane gave 2.2 g (26%) solid.

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. washwashed successively with sodium bicarbonate solution, water, and brine
  3. dry with materialthen dried (Na2SO4)
  4. concentrationand concentrated in vacuo
  5. customto give a solid
  6. customRecrystallization from diethyl ether/pentane