反应 #171199

ord-642d55d22fef44718018b81a798c95bc

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.ADDITIONwas added at 0° C
  2. 2
    其他the reaction mixture was evaporated
  3. 3
    萃取extracted with ethyl acetate
  4. 4
    洗涤The organic layer was washed with water and brine solution
  5. 5
    干燥dried over anhydrous sodium sulphate
  6. 6
    其他The solvent was evaporated under reduced pressure

实验过程

To a solution of the compound obtained from step b above (0.3 g) in tert-butanol:tetrahydrofuran (3 mL:3 mL) at 0° C., a solution of sodium metaperiodate (0.673 g in 3 mL of water) was added. The reaction mixture was stirred for 2 hours at the same temperature and potassium permanganate (0.025 g) was added at 0° C. After stirring the reaction mixture for an additional 6 hours at room temperature, the reaction mixture was evaporated and the residue was taken into water and extracted with ethyl acetate. The organic layer was washed with water and brine solution, and dried over anhydrous sodium sulphate. The solvent was evaporated under reduced pressure, to afford the title compound (0.3 g).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08846910B2uspto-grants-2014_09