ANDROSTA-1,4-DIEN-3-ONE, 17,17-BIS(METHYLTHIO)-9-FLUORO-11-HYDROXY-, (11-beta)- → HCID 14823699、化合物

HRID 372410ノート

反応式

HRID 372410 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][CH2:14][C:15]3(SC)[S:21][CH3:22])[C@@H:11]1[CH2:10][CH2:9][C:8]1[C@:3]2([CH3:26])[CH:4]=[CH:5][C:6](=[O:25])[CH:7]=1>C(C1C=CC=CC=1CC)C>[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([CH3:26])[CH:4]=[CH:5][C:6](=[O:25])[CH:7]=1

参加物

3

反応物 1

HCID 50095ANDROSTA-1,4-DIEN-3-ONE, 17,17-BIS(METHYLTHIO)-9-FLUORO-11-HYDROXY-, (11-beta)-

生成物 1

HCID 14823699HCID 14823699、化合物収率 91.7%

試薬・触媒・溶媒 1

HCID 86571,2-Diethylbenzene溶媒

実験手順

A suspension of 9-fluoro-11β-hydroxy-17,17-bis-(methylthio)androsta-1,4-diene-3-one (3.6 g) in diethylbenzene (250 ml) is slowly distilled from a bath at 220° C. In a few minutes, a clear solution results and the starting material disappears. On cooling in an ice bath, the solution deposits small needles of the analytical specimen of the title compound, (2.9 g), melting point 268° C (dec.). (discoloration starts at 263° C).

後処理

  1. distillationis slowly distilled from a bath at 220° C
  2. waitIn a few minutes
  3. customa clear solution results
  4. temperatureOn cooling in an ice bath

出典と根拠

ORDレコード
ord-fa761554a1524ab9a6abff25e2af2332
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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