반응 #1090362

ord-c904f91c2a4d495885df37eba34b3e90

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과After the catalyst was filtered
  2. 2
    기타the solvent was evaporated at reduced pressure
  3. 3
    기타The residue was purified by column chromatography (silica gel)

실험 절차

To a solution of 3-benzyloxy-17α-tert-butyldimethylsilyloxyestra-1,3,5(10)-triene (50, 1.90 g, 4.0 mmol) in THF (30 mL) was added 10% palladium on carbon (0.500 g). The reaction mixture was stirred for 2 h under a hydrogen atmosphere at room temperature. After the catalyst was filtered, the solvent was evaporated at reduced pressure. The residue was purified by column chromatography (silica gel) using n-hexane:EtOAc (10:1→5:1, v/v) to afford 1.45 g of 51 (94% yield) mp: 161-162° C. (silica gel) using n-hexane:EtOAc (10:1→5:1, v/v) to afford 1.45 g of 51 (94% yield) mp: 161-162° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06046186uspto-grants-2000_04