Water → HCID 18001059、化合物

HRID 1870454ノート

反応式

HRID 1870454 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]([C:12](=[O:22])[C:13]3[CH:18]=[CH:17][C:16]([OH:19])=[C:15]([O:20][CH3:21])[CH:14]=3)[CH2:10][CH2:9][CH2:8][CH2:7][C:6]=2[CH:23]=1.C(=O)([O-])[O-].[K+].[K+].[Cl:30][C:31]1[CH:38]=[CH:37][CH:36]=[CH:35][C:32]=1[CH2:33]Cl.O>CN(C)C=O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]([C:12](=[O:22])[C:13]3[CH:18]=[CH:17][C:16]([O:19][CH2:33][C:32]4[CH:35]=[CH:36][CH:37]=[CH:38][C:31]=4[Cl:30])=[C:15]([O:20][CH3:21])[CH:14]=3)[CH2:10][CH2:9][CH2:8][CH2:7][C:6]=2[CH:23]=1

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 119062-Chlorobenzyl chlorideHCID 18001060HCID 18001060、化合物

生成物 1

HCID 18001059HCID 18001059、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 7-chloro-1-(3-methoxy-4-hydroxybenzoyl)-2,3,4,5-tetrahydro-1H-benzazepine (0.7 g) in dry dimethylformamide (20 ml) are added potassium carbonate (0.35 g) and 2-chlorobenzyl chloride (0.32 ml), and the mixture is stirred at room temperature overnight. To the reaction solution is added water, and the mixture is extracted with ethyl acetate. The extract is washed with water, dried, and evaporated to remove the solvent. The residue is recrystallized from acetone/diethyl ether to give 7-chloro-1-[3-methoxy-4-(2-chlorobenzyloxy)benzoyl]-2,3,4,5-tetrahydro-1H-benzazepine (0.76 g) as white powder.

後処理

  1. extractionthe mixture is extracted with ethyl acetate
  2. washThe extract is washed with water
  3. customdried
  4. customevaporated
  5. customto remove the solvent
  6. customThe residue is recrystallized from acetone/diethyl ether

出典と根拠

ORDレコード
ord-c061b4e29fc24a51ba91d8213fba34ff
出典データセット
uspto-grants-2000_08
特許番号
US06096735

反応ノート

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