반응 #76218
ord-ab8a686577f742cb8dc9fe5a54ecc8c2
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후처리
- 1workup.ADDITIONTo the obtained solution was added dropwise
- 2workup.STIRRINGthe mixture was stirred at room temperature for 1 h
- 3여과The precipitated crystals were collected by filtration
- 4세척washed successively with a 10% aqueous solution of potassium sodium (+)-tartrate tetrahydrate, pure water and isopropyl ether
- 5기타air-dried
실험 절차
Methyl 4-(3,4-dichlorophenyl)-2-(2-methyl-1-imidazolyl)-5-oxazolepropionate (0.67 g) was dissolved in toluene (5 mL). To the obtained solution was added dropwise a mixture of a 70% solution (0.81 g) of sodium bis(2-methoxyethoxy)aluminum hydride in toluene and toluene (2 mL) at 0° C. and the mixture was stirred at 0° C. for 1 h. 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 (0.46 g, 74%). Recrystallization from acetone-hexane gave pale-yellow prism crystals. melting point: 140-141° C.