Aluminum(III) Chloride → HCID 15069388、化合物

HRID 344143

反応式

HRID 344143 の反応式
[Cl-].[Cl-].[Cl-].[Al+3].[CH3:5][CH:6]([CH3:38])[CH2:7][CH2:8][C:9]1[N:13]([CH2:14][C:15]2[CH:20]=[CH:19][C:18]([C:21]3[C:22]([C:27]([OH:29])=[O:28])=[CH:23][CH:24]=[CH:25][CH:26]=3)=[CH:17][CH:16]=2)[C:12]2[CH:30]=[C:31]([O:36][CH3:37])[C:32]([O:34]C)=[CH:33][C:11]=2[N:10]=1>ClCCl>[CH3:5][CH:6]([CH3:38])[CH2:7][CH2:8][C:9]1[N:13]([CH2:14][C:15]2[CH:20]=[CH:19][C:18]([C:21]3[C:22]([C:27]([OH:29])=[O:28])=[CH:23][CH:24]=[CH:25][CH:26]=3)=[CH:17][CH:16]=2)[C:12]2[CH:30]=[C:31]([O:36][CH3:37])[C:32]([OH:34])=[CH:33][C:11]=2[N:10]=1

参加物

4

反応物 2

HCID 6451240Aluminum(III) ChlorideHCID 150693604'-[(2-(3-Methylbutyl)-5,6-dimethoxy-benzimidazol-1-yl)-methyl]biphenyl-2-carboxylic acid

生成物 1

HCID 15069388HCID 15069388、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

3 g of aluminium trichloride are added to a suspension of 600 mg (1.3 mmol) of 4'-[(2-(3-methylbutyl)-5,6-dimethoxy-benzimidazol-1-yl)-methyl]biphenyl-2-carboxylic acid in 50 ml of dry dichloromethane and the mixture is heated under reflux for 15 minutes. The solvent is then distilled off, the residue is filtered off under suction, washed using 30 ml of water and dried. 360 mg (62% of theoretical) of a mixture of the isomeric products is obtained after chromatographing over silica gel (eluting agent: dichloromethane/ethanol=9:1).

後処理

  1. temperaturethe mixture is heated
  2. temperatureunder reflux for 15 minutes
  3. distillationThe solvent is then distilled off
  4. filtrationthe residue is filtered off under suction
  5. washwashed
  6. customdried
  7. addition360 mg (62% of theoretical) of a mixture of the isomeric products
  8. customis obtained after chromatographing over silica gel (eluting agent: dichloromethane/ethanol=9:1)

出典と根拠

ORDレコード
ord-ab3b77ca0d30432a9ebac45cccfa1e26
出典データセット
uspto-grants-1999_01
特許番号
US05864043

関連ノート

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