تفاعل #94828

ord-4e98e46d8be14dc0b62c0c3aef402f49

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىis brought to 20°-25°
  2. 2
    أخرىThe layers are separated
  3. 3
    استخلاصthe aqueous layer is extracted with methylene chloride (2×5 ml)
  4. 4
    غسيلwashed with water (10 ml)
  5. 5
    تجفيفdried over sodium sulfate
  6. 6
    تركيزconcentrated under reduced pressure

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04342702uspto-grants-1982_08