m-Chloroperbenzoic acid → HCID 14823693、化合物

HRID 372411ノート

反応式

HRID 372411 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 (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.

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-a9c08ff645414180ad6d20aea18cc714
出典データセット
uspto-grants-1978_05
特許番号
US04091036

反応ノート

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