HRID2177686
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customwas sealed under nitrogen in a microwave vial
- temperatureAfter cooling
- filtrationthe solid was filtered off
- customThe filtrate was evaporated to dryness
- customthe residue was purified by HPLC
- washeluting with a mixture of methanol and water containing 0.1% formic acid with a gradient of 20-98%