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

HRID 839464ノート

反応式

HRID 839464 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-41cd34b67e4f494bb5105c2a9d0d5950
出典データセット
uspto-grants-1978_06
特許番号
US04094840

反応ノート

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