HRID1393074
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
PROCEDURE
实验过程
A solution of crude (2-methyl-4-{methyl-[4-methyl-2-(4-trifluoromethyl-phenyl)-thiazol-5-ylmethyl]-amino}-phenoxy)-acetic acid ethyl ester (0.84 g containing 0.74 g, 1.54 mmol) in THF/EtOH (9.2 ml, 1:1) were treated at 0° C. with 1M LiOH (4.6 ml, 4.6 mmol) for 2 min. After 2 h at RT, the solution was acidified by adding aqueous 10% KHSO4, and the mixture was extracted with Et2O (3×). The organic phase was washed with aqueous 10% NaCl, dried over Na2SO4 and evaporated. Crystallization (CH2Cl2/Et2O) gave 0.57 g (82%) (2-methyl-4-{methyl-[4-methyl-2-(4-trifluoromethyl-phenyl)-thiazol-5-ylmethyl]-amino}-phenoxy)-acetic acid as light yellow powder, MS: 449 (M-H)−, MP: 146-149° C., dec.
WORKUP
后处理
- extractionthe mixture was extracted with Et2O (3×)
- washThe organic phase was washed with aqueous 10% NaCl
- dry with materialdried over Na2SO4
- customevaporated
- customCrystallization (CH2Cl2/Et2O)