HRID1745786
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
- 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
- extractionThe mixture was extracted with ethyl acetate
- washthe organic layer was washed successively with H2O, sat. Na2CO3-sol
- dry with materialand brine, dried over Na2SO4
- customevaporated in vacuum
- customThe residue was triturated with ethyl acetate