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

HRID 372410Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 372410
[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

Komponenten

3

Edukt 1

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

Produkt 1

HCID 14823699HCID 14823699, VerbindungAusbeute 91,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 86571,2-DiethylbenzeneLösungsmittel

Versuchsvorschrift

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).

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-fa761554a1524ab9a6abff25e2af2332
Quelldatensatz
uspto-grants-1978_05
Patentnummer
US04091036

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