Nimodipine → Dehydro nimodipine

HRID 615181

Reaktionsgleichung

Reaktionsgleichung von HRID 615181
[CH3:1][C:2]1[NH:3][C:4]([CH3:30])=[C:5]([C:23]([O:25][CH2:26][CH2:27][O:28][CH3:29])=[O:24])[CH:6]([C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([N+:20]([O-:22])=[O:21])[CH:15]=2)[C:7]=1[C:8]([O:10][CH:11]([CH3:13])[CH3:12])=[O:9]>C(O)(=O)C.[O-2].[Cr+6].[O-2].[O-2]>[CH3:1][C:2]1[C:7]([C:8]([O:10][CH:11]([CH3:13])[CH3:12])=[O:9])=[C:6]([C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([N+:20]([O-:22])=[O:21])[CH:15]=2)[C:5]([C:23]([O:25][CH2:26][CH2:27][O:28][CH3:29])=[O:24])=[C:4]([CH3:30])[N:3]=1

Komponenten

4

Edukt 1

HCID 4497Nimodipine

Produkt 1

HCID 529928Dehydro nimodipine

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 10219390chromium (VI) trioxideKatalysatorHCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

6.8 g of chromium(VI) oxide were added in portions to a boiling solution of 41.8 g (100 mmols) of isopropyl 2-methoxyethyl 1,4-dihydro-2,6-dimethyl-4-(3-nitrophenyl)pyridine-3,5-dicarboxylate in 160 ml of glacial acetic acid. The mixture was then heated under reflux for a further 30 minutes and, after cooling down, poured into ammoniacal ice-water. The mixture was extracted with chloroform and the extracts, after drying over sodium sulphate, were evaporated in vacuo. 35.9 g (86% of theory) of an oil resulted.

Aufarbeitung

  1. temperatureThe mixture was then heated
  2. temperatureunder reflux for a further 30 minutes
  3. temperatureafter cooling down
  4. extractionThe mixture was extracted with chloroform
  5. dry with materialthe extracts, after drying over sodium sulphate
  6. customwere evaporated in vacuo
  7. custom35.9 g (86% of theory) of an oil resulted

Quellen und Nachweise

ORD-Eintrag
ord-0e7c6c54a4514adca34d6ba6b65b0a33
Quelldatensatz
uspto-grants-1985_02
Patentnummer
US04497821

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