HRID2044025

反应详情

EQUATION

反应方程式

HRID 2044025 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
35 °C

PROCEDURE

实验过程

The mixture of ethyl (3E)-3-(2,2-dimethyl-1,3-dioxolan-4-ylidene)-2-oxopropanoate (21.4 g, 0.1 mol) and 2-hydrazino-3-chloropyridine (14.3 g, 0.1 mol) in 50 ml of ethanol was stirred for 18 hours at 35° C. Ethanol was removed in vacuo and the residue was taken up in 100 ml of methyl (tert)-butyl ether. The organic phase was washed once with 50 ml of 1% strength HCl and concentrated by evaporation. This gave 26.2 g (86% yield) of the product as a viscous oil with a purity (HPLC) of 97%.

WORKUP

后处理

  1. customEthanol was removed in vacuo
  2. washThe organic phase was washed once with 50 ml of 1% strength HCl
  3. concentrationconcentrated by evaporation