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Dimethylformamide → 5-[4-(3,4-Dimethoxybenzyl)-1-piperazinyl]-3,4-dihydrocarbostyril dihydrochloride

HRID 1649223
ノート
印刷プレビュー

反応式

HRID 1649223 の反応式
[N:1]1([C:7]2[CH:16]=[CH:15][CH:14]=[C:13]3[C:8]=2[CH2:9][CH2:10][C:11](=[O:17])[NH:12]3)[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.C(=O)([O-])[O-].[K+].[K+].CN(C=O)C.[CH3:29][O:30][C:31]1[CH:32]=[C:33]([CH:36]=[CH:37][C:38]=1[O:39][CH3:40])[CH2:34][Cl:35]>O>[ClH:35].[ClH:35].[CH3:29][O:30][C:31]1[CH:32]=[C:33]([CH:36]=[CH:37][C:38]=1[O:39][CH3:40])[CH2:34][N:4]1[CH2:5][CH2:6][N:1]([C:7]2[CH:16]=[CH:15][CH:14]=[C:13]3[C:8]=2[CH2:9][CH2:10][C:11](=[O:17])[NH:12]3)[CH2:2][CH2:3]1
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 4

HCID 6228DimethylformamideHCID 11430Potassium CarbonateHCID 81740Veratryl chlorideHCID 11630008HCID 11630008、化合物

生成物 1

HCID 204805935-[4-(3,4-Dimethoxybenzyl)-1-piperazinyl]-3,4-dihydrocarbostyril dihydrochloride収率 58.4%

試薬・触媒・溶媒 1

HCID 962
Water
溶媒

実験手順

To a mixture of 1.2 g of 5-(1-piperazinyl)-3,4-dihydrocarbostyril, 1.17 g of potassium carbonate and 20 ml of DMF was added 858 mg of 3,4-dimethoxybenzyl chloride and the mixture was stirred at 70°-80° C. for 2 hours. The reaction mixture was poured into a large amount of water and extracted with chloroform. After washing with water the extract was dried over anhydrous sodium sulfate. Chloroform was distilled off and the residue was purified through silica gel column chromatography. The residue was converted to hydrochloric acid salt to give 610 mg of 5-[4-(3,4-dimethoxybenzyl)-1-piperazinyl]-3,4-dihydrocarbostyril dihydrochloride, m.p. 270°-272.5° C. (decomp.).

後処理

  1. extractionextracted with chloroform
  2. washAfter washing with water the extract
  3. dry with materialwas dried over anhydrous sodium sulfate
  4. distillationChloroform was distilled off
  5. customthe residue was purified through silica gel column chromatography

出典と根拠

ORDレコード
ord-d7ad9643f748485eaee173de2e81b7b1
出典データセット
uspto-grants-1983_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04415572

反応ノート

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