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Dimethylformamide → 5-[4-(3,4-Dichlorobenzyl)-1-piperazinyl]-3,4-dihydrocarbostyril monohydrochloride monohydrate

HRID 1649225
ノート
印刷プレビュー

反応式

HRID 1649225 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.[Cl:29][C:30]1[CH:31]=[C:32]([CH:35]=[CH:36][C:37]=1[Cl:38])[CH2:33]Cl>O>[OH2:17].[ClH:29].[Cl:29][C:30]1[CH:31]=[C:32]([CH:35]=[CH:36][C:37]=1[Cl:38])[CH2:33][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 76093,4-Dichlorobenzyl chlorideHCID 11430Potassium CarbonateHCID 11630008HCID 11630008、化合物

生成物 1

HCID 204805885-[4-(3,4-Dichlorobenzyl)-1-piperazinyl]-3,4-dihydrocarbostyril monohydrochloride monohydrate収率 16.7%

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 895 mg of 3,4-dichlorobenzyl chloride and the mixture was stirred at 60°-70° C. for 3 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. After conversion to hydrochloric acid salt with methanol-hydrochloric acid the product was recrystallized from methanol to give 0.17 g of 5-[4-(3,4-dichlorobenzyl)-1-piperazinyl]-3,4-dihydrocarbostyril monohydrochloride monohydrate, m.p. 298.5°-300° C. (decomp.), colorless granules.

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
  6. customAfter conversion to hydrochloric acid salt with methanol-hydrochloric acid the product was recrystallized from methanol

出典と根拠

ORDレコード
ord-476273bcdc8f475f916eda529d7f7259
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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