HRID1427157

反应详情

EQUATION

反应方程式

HRID 1427157 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a suspension of 4-chloro-3-pyridinecarboxylic acid (3.630 g) in dichloromethane (20 mL) and methanol (8 mL) stirred under argon at 0° C. was added TMS-diazomethane 2M in Et2O (17.28 mL) dropwise. The reaction mixture was stirred at room temperature for 1 h. The solvents were evaporated in vacuo and the crude product was added to a silica gel column and was eluted with cyclohexane/EtOAc=7/3. The evaporation of the collected fractions gave 2.7 g of the title compound as a colourless solid.

WORKUP

后处理

  1. stirringThe reaction mixture was stirred at room temperature for 1 h
  2. customThe solvents were evaporated in vacuo
  3. additionthe crude product was added to a silica gel column
  4. washwas eluted with cyclohexane/EtOAc=7/3
  5. customThe evaporation of the collected fractions