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Water → 5-[4-(4-Methoxybenzoyl)-1-piperazinyl]-3,4-dihydrocarbostyril

HRID 1649211
ノート
印刷プレビュー

反応式

HRID 1649211 の反応式
Br.[N:2]1([C:8]2[CH:17]=[CH:16][CH:15]=[C:14]3[C:9]=2[CH2:10][CH2:11][C:12](=[O:18])[NH:13]3)[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.C(N(CC)CC)C.[CH3:26][O:27][C:28]1[CH:36]=[CH:35][C:31]([C:32](Cl)=[O:33])=[CH:30][CH:29]=1.O>CN(C=O)C>[CH3:26][O:27][C:28]1[CH:36]=[CH:35][C:31]([C:32]([N:5]2[CH2:6][CH2:7][N:2]([C:8]3[CH:17]=[CH:16][CH:15]=[C:14]4[C:9]=3[CH2:10][CH2:11][C:12](=[O:18])[NH:13]4)[CH2:3][CH2:4]2)=[O:33])=[CH:30][CH:29]=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 962WaterHCID 7477p-Anisoyl chlorideHCID 8471TriethylamineHCID 204805915-(1-Piperazinyl)-3,4-dihydrocarbostyril monohydrobromide

生成物 1

HCID 132363425-[4-(4-Methoxybenzoyl)-1-piperazinyl]-3,4-dihydrocarbostyril収率 36.1%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒
2 回

実験手順

5-(1-Piperazinyl)-3,4-dihydrocarbostyril monohydrobromide (2.6 g) and 2.34 ml of triethylamine were dissolved in 40 ml of DMF. The mixture was stirred at room temperature while slowly adding dropwise 10 ml of DMF solution containing 2.5 g of 4-methoxybenzoyl chloride. After completion of addition the reaction mixture was stirred for 30 minutes. The reaction mixture was poured into a large amount of water and extracted with chloroform. The extract was washed with saturated sodium hydrogencarbonate solution and subsequently with water and dried over anhydrous sodium sulfate. Chloroform was distilled off and residual crystals were recrystallized from methanol-chloroform to give 1.1 g of 5-[4-(4-methoxybenzoyl)-1-piperazinyl]-3,4-dihydrocarbostyril, m.p. 219°-220° C., colorless needles.

後処理

  1. additionAfter completion of addition the reaction mixture
  2. stirringwas stirred for 30 minutes
  3. extractionextracted with chloroform
  4. washThe extract was washed with saturated sodium hydrogencarbonate solution and subsequently with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationChloroform was distilled off
  7. customresidual crystals were recrystallized from methanol-chloroform

出典と根拠

ORDレコード
ord-b96a25f375e547de96f3ce2f53ef1fdd
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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