m-Chloroperbenzoic acid → HCID 14823693、化合物

HRID 614997ノート

反応式

HRID 614997 の反応式
[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

参加物

4

反応物 2

HCID 70297m-Chloroperbenzoic acidHCID 14823699HCID 14823699、化合物

生成物 1

HCID 14823693HCID 14823693、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

To a stirred solution of 1.0 g of 9-fluoro-11β-hydroxy-17-(methylthio)androsta-1,4,16-trien-3-one in chloroform (500 ml) is added a solution of 85% m-chloroperbenzoic acid (552 mg) in chloroform (100 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.

後処理

  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

出典と根拠

ORDレコード
ord-410fbda8e0104a0a9f99c6e4878af727
出典データセット
uspto-grants-1979_03
特許番号
US04146538

反応ノート

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