HRID1476913

反应详情

EQUATION

反应方程式

HRID 1476913 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
160 °C

PROCEDURE

实验过程

A mixture of 6-chloro-4-methylpicolinonitrile (3 g, 19.66 mmol) and ethyl hydrazinecarboxylate (8.19 g, 79 mmol) in NMP (6 mL) was heated in a sealed tube at 160° C. overnight. The residue was purified by column chromatography eluting with a gradient of 0-80% EtOAc in heptanes. The product-containing fractions were collected and evaporated in vacuo to give the title compound as a yellow semi-solid (428 mg). ESI-MS m/z [M+H]+211.6.

WORKUP

后处理

  1. customThe residue was purified by column chromatography
  2. washeluting with a gradient of 0-80% EtOAc in heptanes
  3. customThe product-containing fractions were collected
  4. customevaporated in vacuo