反应 #43905

ord-0fc48cb907c544e4a4e86b869454a751

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度cooling
  2. 2
    workup.STIRRINGthe mixture was stirred at room temperature for 1 hr
  3. 3
    过滤The insoluble substance was filtered off through celite
  4. 4
    浓缩the filtrate was concentrated under reduced pressure

实验过程

To a solution of methyl 4′-[(1,1-dioxidotetrahydro-2H-thiopyran-4-yl)oxy]-2′,6′-dimethylbiphenyl-3-carboxylate (0.128 g, 0.33 mmol) in tetrahydrofuran (2 mL) was added lithium aluminum hydride (80%, 15.7 mg, 0.33 mmol) by small portions under ice-cooling, and the mixture was stirred at the same temperature for 1.5 hr. Sodium sulfate 10 hydrate (0.106 g, 0.33 mmol) was added by small portions to the reaction mixture, and the mixture was stirred at room temperature for 1 hr. The insoluble substance was filtered off through celite, and the filtrate was concentrated under reduced pressure to give the title compound (0.111 g, yield 93%) as a colorless amorphous powder.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07732626B2uspto-grants-2010_06