HRID2177686

反应详情

EQUATION

反应方程式

HRID 2177686 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
160 °C

PROCEDURE

实验过程

A mixture of 6-(benzenesulphonylmethyl)-3-bromo-2-methoxybenzoic acid (Intermediate 133, 0.20 g), copper (I) oxide (0.008 g), salicylaldoxime (0.032 g), imidazole (0.08 g), cesium carbonate (0.5 g) in acetonitrile (4 ml) was sealed under nitrogen in a microwave vial and heated at 160° C. for 1 hour. After cooling, ethyl acetate was added and the solid was filtered off. The filtrate was evaporated to dryness and the residue was purified by HPLC, eluting with a mixture of methanol and water containing 0.1% formic acid with a gradient of 20-98% to give 6-benzenesulphonylmethyl-3-(imidazol-1-yl)-2-methoxybenzoic acid as a white solid.

WORKUP

后处理

  1. customwas sealed under nitrogen in a microwave vial
  2. temperatureAfter cooling
  3. filtrationthe solid was filtered off
  4. customThe filtrate was evaporated to dryness
  5. customthe residue was purified by HPLC
  6. washeluting with a mixture of methanol and water containing 0.1% formic acid with a gradient of 20-98%