반응 #94829

ord-846a8806a8f34412a7df715c710e35fc

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도the resulting slurry heated at 40° for 1.5 hours
  2. 2
    온도The mixture is cooled to 20°-25°
  3. 3
    기타The solids are isolated by filtration
  4. 4
    세척washed with hexane/ethyl acetate (85/15, 13 ml)

실험 절차

21-Chloro-17α-hydroxy-20-methoxypregna-4,9(11),20-trien-3-one (VII, Example 4, 1.0 g), THF (4 ml), acetone (4.9 ml), and methanol (1.4 ml) are mixed. Aqueous hydrochloric acid (6 N, 0.44 ml) is added and the resulting slurry heated at 40° for 1.5 hours. The mixture is cooled to 20°-25° and diluted with hexane (3 ml). The solids are isolated by filtration and washed with hexane/ethyl acetate (85/15, 13 ml) to give the title compound.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04342702uspto-grants-1982_08