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Ethanol → HCID 9822781、化合物

HRID 1736407
ノート
印刷プレビュー

反応式

HRID 1736407 の反応式
C(O)C.[N+:4]([C:7]1[CH:17]=[CH:16][C:15]([O:18][CH2:19][CH2:20][CH2:21][S:22]([C:24]2[N:25]([C:29]3[CH:34]=[CH:33][CH:32]=[CH:31][C:30]=3[CH3:35])[CH:26]=[CH:27][N:28]=2)=[O:23])=[CH:14][C:8]=1[CH:9]=[CH:10][C:11](O)=[O:12])([O-])=O.[H][H]>[C].[Pd].C(N(CC)CC)C>[CH3:35][C:30]1[CH:31]=[CH:32][CH:33]=[CH:34][C:29]=1[N:25]1[CH:26]=[CH:27][N:28]=[C:24]1[S:22]([CH2:21][CH2:20][CH2:19][O:18][C:15]1[CH:14]=[C:8]2[C:7](=[CH:17][CH:16]=1)[NH:4][C:11](=[O:12])[CH2:10][CH2:9]2)=[O:23]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 702EthanolHCID 53900945HCID 53900945、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 9822781HCID 9822781、化合物収率 26%

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 8471Triethylamine溶媒

実験手順

To 50 ml of ethanol were added 300 mg of 2-nitro-5-{3-[1-(2-methylphenyl)-2-imidazolylsulfinyl]-propoxy}cinnamic acid, 100 mg of 10% palladium carbon and 0.6 ml of triethylamine. Hydrogenation was conducted at a hydrogen pressure of 4 atm. at 60° C. for 3 hours. The reaction mixture was cooled to room temperature and filtered to remove the catalyst. To the filtrate was added 200 mg of 10% palladium carbon, and hydrogenation was conducted at a hydrogen pressure of 4 atm. at 60° C. for 6 hours. Ethanol was removed by distillation. The residue was made acidic with hydrochloric acid, followed by extraction with methylene chloride. The extract was washed with an aqueous solution saturated with sodium chloride, dried with anhydrous magnesium sulfate, and subjected to distillation to remove the solvent. The residue was purified by a silica gel column chromatography (eluant: dichloromethane/methanol=50/1→20/1). The crude crystals were recrystallized from ethanol-n-hexane to obtain 70 mg of 6-{3-[1-(2-methylphenyl)-2-imidazolylsulfinyl]propoxy}-3,4-dihydrocarbostyril.

後処理

  1. filtrationfiltered
  2. customto remove the catalyst
  3. additionTo the filtrate was added 200 mg of 10% palladium carbon, and hydrogenation
  4. customEthanol was removed by distillation
  5. extractionfollowed by extraction with methylene chloride
  6. washThe extract was washed with an aqueous solution saturated with sodium chloride
  7. dry with materialdried with anhydrous magnesium sulfate
  8. distillationsubjected to distillation
  9. customto remove the solvent
  10. customThe residue was purified by a silica gel column chromatography (eluant: dichloromethane/methanol=50/1→20/1)
  11. customThe crude crystals were recrystallized from ethanol-n-hexane

出典と根拠

ORDレコード
ord-faaaae4446624973bf409163554d0a2c
出典データセット
uspto-grants-1996_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05541198

反応ノート

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