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Nimodipine → Dehydro nimodipine

HRID 615181
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HRID 615181 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 4497Nimodipine

생성물 1

HCID 529928Dehydro nimodipine

시약·촉매·용매 2

HCID 10219390chromium (VI) trioxide촉매HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0e7c6c54a4514adca34d6ba6b65b0a33
출처 데이터셋
uspto-grants-1985_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04497821

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