Nimodipine → Dehydro nimodipine

HRID 615181

反応式

HRID 615181 の反応式
[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

参加物

4

反応物 1

HCID 4497Nimodipine

生成物 1

HCID 529928Dehydro nimodipine

試薬・触媒・溶媒 2

HCID 10219390chromium (VI) trioxide触媒HCID 176Acetic Acid溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-0e7c6c54a4514adca34d6ba6b65b0a33
出典データセット
uspto-grants-1985_02
特許番号
US04497821

関連ノート

読み込み中…