HRID1515371

反应详情

EQUATION

反应方程式

HRID 1515371 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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 (21.4 g, 0.15 mol) in 150 ml of ethanol was stirred for 8 hours at RT. Ethanol was removed in vacuo and the residue was taken up in 200 ml of methyl tert-butyl ethyl. The organic phase was washed three times with in each case 50 ml of 1% HCl and concentrated by evaporation. This gave 36 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 three times with in each case 50 ml of 1% HCl
  3. concentrationconcentrated by evaporation