HRID401762

反应详情

EQUATION

反应方程式

HRID 401762 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of methyl 4-{[(2,4-dimethoxybenzyl)(1,3-thiazol-2-yl)amino]sulfonyl}-2-fluorobenzoate (Preparation 14, 10 g, 21 mmol, 1 eq) and sodium hydroxide 4.3 g, 0.107 mol, 5 eq) in THF: MeOH: water (25 ml:2 ml:75 ml) was heated at 50° C. for 4 hours. The reaction mixture was acidified to pH 2.0 with 2M HCl and the resulting precipitate collected by filtration. The crude material was purified by column chromatography eluting with 90:10:1 DCM: MeOH: ammonia to yield the title compound as a yellow solid (706 mg, 2.33 mmol, 11%).

WORKUP

后处理

  1. filtrationthe resulting precipitate collected by filtration
  2. customThe crude material was purified by column chromatography
  3. washeluting with 90:10:1 DCM