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
- 0 °C
PROCEDURE
实验过程
Methyl 2-(2-methyl-1-imidazolyl)-4-(4-trifluoromethylphenyl)-5-oxazolepropionate (1.00 g) was dissolved in toluene (15 mL). To the obtained solution was added dropwise a mixture of a 70% solution (1.20 g) of sodium bis(2-methoxyethoxy)aluminum hydride in toluene and toluene (5 mL) at 0° C., and the mixture was stirred at 0° C. for 30 min. To the reaction mixture was carefully added a 10% aqueous solution (50 mL) of potassium sodium (+)-tartrate tetrahydrate, and the mixture was stirred at room temperature for 1 h. The precipitated crystals were collected by filtration, washed successively with a 10% aqueous solution of potassium sodium (+)-tartrate tetrahydrate, pure water and isopropyl ether, and air-dried to give the title compound as crystals (0.75 g, 81%). Recrystallization from ethyl acetate-isopropyl ether gave pale-yellow prism crystals. melting point: 127-129° C.
WORKUP
后处理
- additionTo the obtained solution was added dropwise
- stirringthe mixture was stirred at room temperature for 1 h
- filtrationThe precipitated crystals were collected by filtration
- washwashed successively with a 10% aqueous solution of potassium sodium (+)-tartrate tetrahydrate, pure water and isopropyl ether
- customair-dried