HRID2261737

反应详情

EQUATION

反应方程式

HRID 2261737 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
105 °C

PROCEDURE

实验过程

A mixture of 3-acetyl-2-methoxyimino-5-methyl-hexanoic acid ethyl ester (1 g, 4.1 mmol), 2,6-dichlorophenylhydrazine hydrochloride (1.76 g, 8.2 mmol) in glacial acetic acid (10 mL) and 2-methoxy-ethanol (5 mL) is stirred at 105° C. for 3 hours. The reaction is concentrated and the residue is partitioned between EtOAc and 1N HCl. The organic layer is concentrated and purified by column chromatography (0-20% EtOAc in hexanes) to give the title product as an oil, 1.1 g (76%).

WORKUP

后处理

  1. concentrationThe reaction is concentrated
  2. customthe residue is partitioned between EtOAc and 1N HCl
  3. concentrationThe organic layer is concentrated
  4. custompurified by column chromatography (0-20% EtOAc in hexanes)