反应 #94828

ord-4e98e46d8be14dc0b62c0c3aef402f49

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他is brought to 20°-25°
  2. 2
    其他The layers are separated
  3. 3
    萃取the aqueous layer is extracted with methylene chloride (2×5 ml)
  4. 4
    洗涤washed with water (10 ml)
  5. 5
    干燥dried over sodium sulfate
  6. 6
    浓缩concentrated under reduced pressure

实验过程

To a solution of 21-chloro-20-methoxy-21-(phenylsulfinyl)pregna-4,9(11),17(20)-trien-3-one (VI, Example 3, 100 mg) in THF (2 ml), methanol (0.45 ml) and acetone (0.3 ml) at 0° under nitrogen is added a solution of sodium hydroxide (5 N, 0.04 ml). The mixture is brought to 20°-25° and is allowed to stir for 24 hr. The mixture is poured into a mixture of water (25 ml) and methylene chloride (10 ml). The layers are separated and the aqueous layer is extracted with methylene chloride (2×5 ml). The organic extracts are combined and washed with water (10 ml), dried over sodium sulfate and concentrated under reduced pressure to give the title compound.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04342702uspto-grants-1982_08