HRID1062250

反应详情

EQUATION

反应方程式

HRID 1062250 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
23 °C

PROCEDURE

实验过程

To a solution of 2-{3-[7-(4-fluoro-phenyl)-4-oxo-4,5-dihydro-3H-benzo[b][1,4]diazepin-2-yl]-phenyl}-thiazole-4-carboxylic acid ethyl ester (Example 153) (49 mg, 0.1 mmol) in a mixture of MeOH (1 mL) and DMSO (1.5 mL) was added 2N KOH (1 mL, 2 mmol). The mixture was stirred at 23° C. for 0.5 h and then partitioned between ethyl acetate and H2O. The pH of the aqueous phase was set to 3 by the addition of 3N HCl and then stirred in the ice-bath for 0.5 h. The precipitate was collected by filtration, triturated with EtOH/Et2O (1/1) and dried, to give the title compound as light yellow solid (25 mg).

WORKUP

后处理

  1. custompartitioned between ethyl acetate and H2O
  2. additionThe pH of the aqueous phase was set to 3 by the addition of 3N HCl
  3. stirringstirred in the ice-bath for 0.5 h
  4. filtrationThe precipitate was collected by filtration
  5. customtriturated with EtOH/Et2O (1/1)
  6. customdried