HRID1062249

反应详情

EQUATION

反应方程式

HRID 1062249 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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) (110 mg, 0.23 mmol) in THF (7 mL) was added a 3.5 M solution of sodium dihydrido-bis(2-methoxyethoxy)aluminate in toluene(0.66 mL, 2.3 mmol). The raction mixture was stirred at 23° C. for 15 min. and then poured into ice-cold 10% aq. acetic acid. The mixture was extracted with ethyl acetate and the organic layer was washed successively with H2O, sat. Na2CO3-sol. and brine, dried over Na2SO4 and evaporated in vacuum. The residue was triturated with ethyl acetate to give the title compound as light yellow solid (48 mg).

WORKUP

后处理

  1. extractionThe mixture was extracted with ethyl acetate
  2. washthe organic layer was washed successively with H2O, sat. Na2CO3-sol
  3. dry with materialand brine, dried over Na2SO4
  4. customevaporated in vacuum
  5. customThe residue was triturated with ethyl acetate