Water → HCID 86746635, Verbindung

HRID 1613970

Reaktionsgleichung

Reaktionsgleichung von HRID 1613970
O.[C:2]([O:5][CH2:6][CH:7]([N+:32]([O-])=[O:33])[C:8]1[C@:25]2([CH3:26])[C@H:11]([C@H:12]3[C@:22]([OH:27])([CH2:23][CH2:24]2)[C@:20]2([CH3:21])[C:15]([CH2:16][C:17]4(OCC[O:28]4)[CH2:18][CH2:19]2)=[CH:14][CH2:13]3)[CH2:10][CH:9]=1)(=[O:4])[CH3:3].[Cl-].[Na+]>CC(C)=O.[Cr](Cl)(Cl)=O.[Cl-].[Cr+2].[Cl-].[Zn]>[C:2]([O:5][CH2:6][C:7](=[N:32][OH:33])[C:8]1[C@:25]2([CH3:26])[C@H:11]([C@H:12]3[C@:22]([OH:27])([CH2:23][CH2:24]2)[C@:20]2([CH3:21])[C:15](=[CH:16][C:17](=[O:28])[CH2:18][CH2:19]2)[CH2:14][CH2:13]3)[CH2:10][CH:9]=1)(=[O:4])[CH3:3]

Komponenten

8

Edukt 3

HCID 962WaterHCID 5234Sodium ChlorideHCID 57121005HCID 57121005, Verbindung

Produkt 1

HCID 86746635HCID 86746635, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 4

HCID 23994ZincKatalysatorHCID 10197677chromium(II) dichlorideKatalysatorHCID 178526110HCID 178526110, VerbindungKatalysatorHCID 180AcetoneLösungsmittel

Versuchsvorschrift

A filtered aqueous solution of chromous chloride, prepared from chromium (II) chloride (26.1 g), water (121.8 ml) concentrated hydrochloric acid (52.2 ml) and zinc powder (15.7 g) according to the method of J. R. Hanson and T. D. Organ; J. Chem. Soc.(C) 1970, 1182, was added under nitrogen to a stirred solution of 21-acetoxy-3,3-ethylenedioxy-20-nitropregna-5,16-dien-9α-ol (8.70 g as a mixture of 2 diastereomers) in acetone (1.3 1). After stirring for 45 seconds the reaction mixture was poured into an aqueous sodium chloride solution. The resulting layers were separated after which the aqueous layer was washed twice with diethyl ether (400 ml). The combined organic layers were washed once with aqueous sodium chloride solution (450 ml), dried and evaporated under reduced pressure to afford the title compound.

Aufarbeitung

  1. customThe resulting layers were separated after which the aqueous layer
  2. washwas washed twice with diethyl ether (400 ml)
  3. washThe combined organic layers were washed once with aqueous sodium chloride solution (450 ml)
  4. customdried
  5. customevaporated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-a11b45a2e8524fbb9a9e15d107021bf3
Quelldatensatz
uspto-grants-1993_03
Patentnummer
US05194602

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