反应 #1702120
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08188097B2
反应条件: temp:120.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A mixture of (R)-methioninol (4.95 g), benzonitrile (8.3 mL) and zinc bromide (250 mg) was stirred at 120° C. for 90 hours under nitrogen gas atmosphere. After cooling to room temperature, the reaction mixture was filtered and the filtrate was washed with water and a brine, dried over magnesium sulfate and filtered again. The filtrate was concentrated in vacuo and the resultant crude product was purified by a column chromatography on silica gel (solvent; hexane/ethyl acetate=5/1 to 3/1) to give (R)-4-(2-methylthioethyl)-2-phenyl-4,5-dihydrooxazole (3.94 g, yield: 48.6%) as a colorless oil. After cooling to room temperature the reaction mixture was filtered the filtrate was washed with water a brine, dried over magnesium sulfate filtered again The filtrate was concentrated in vacuo the resultant crude product was purified by a column chromatography on silica gel (solvent; hexane/ethyl acetate=5/1 to 3/1)
来源 ID: ord-447f02eb0082426faa912d1d62a8f496