반응 #76218

ord-ab8a686577f742cb8dc9fe5a54ecc8c2

반응 조건

온도
0°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONTo the obtained solution was added dropwise
  2. 2
    workup.STIRRINGthe mixture was stirred at room temperature for 1 h
  3. 3
    여과The precipitated crystals were collected by filtration
  4. 4
    세척washed successively with a 10% aqueous solution of potassium sodium (+)-tartrate tetrahydrate, pure water and isopropyl ether
  5. 5
    기타air-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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06699995B1uspto-grants-2004_03