m-Chloroperbenzoic acid → HCID 14823693, 화합물

HRID 839468노트

반응식

HRID 839468 반응식
[F:1][C@:2]12[C@@H:19]([OH:20])[CH2:18][C@@:16]3([CH3:17])[C@@H:12]([CH2:13][CH:14]=[C:15]3[S:21][CH3:22])[C@@H:11]1[CH2:10][CH2:9][C:8]1[C@:3]2([CH3:24])[CH:4]=[CH:5][C:6](=[O:23])[CH:7]=1.ClC1C=CC=C(C(OO)=[O:33])C=1>C(Cl)(Cl)Cl>[F:1][C@:2]12[C@@H:19]([OH:20])[CH2:18][C@@:16]3([CH3:17])[C@@H:12]([CH2:13][CH:14]=[C:15]3[S:21]([CH3:22])=[O:33])[C@@H:11]1[CH2:10][CH2:9][C:8]1[C@:3]2([CH3:24])[CH:4]=[CH:5][C:6](=[O:23])[CH:7]=1

참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 14823699HCID 14823699, 화합물

생성물 1

HCID 14823693HCID 14823693, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

To a stirred solution of 1.0 g of 9-fluoro-11β-hydroxy-17-(methylthio)androsta-1,4,16-trien-3-one (see Example 1B) in chloroform (500 ml) is added a solution of 85% m-chloroperbenzoic acid (552 mg) in chloroform (10 ml) in the course of 3.0 minutes. In less than 10 minutes, the peracid and the starting steroid disappear. The solution is then washed with a dilute potassium carbonate solution and water, dried, concentrated (to about 10 ml) and diluted with ethyl acetate resulting in the precipitation of small, light needles of the analytical specimen of the title compound, (1.0 g), melting point 268°-269° C (dec.). This is a mixture of the two sulfinyl isomers.

후처리

  1. waitIn less than 10 minutes
  2. washThe solution is then washed with a dilute potassium carbonate solution and water
  3. customdried
  4. concentrationconcentrated (to about 10 ml)
  5. additiondiluted with ethyl acetate resulting in the precipitation of small, light needles of the analytical specimen of the title compound, (1.0 g), melting point 268°-269° C (dec.)
  6. additiona mixture of the two sulfinyl isomers

출처 및 근거

ORD 기록
ord-6032082f92f44cf78ce50e71de34d90a
출처 데이터셋
uspto-grants-1978_06
특허 번호
US04094840

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