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

HRID 1649211
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HRID 1649211 반응식
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
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참가 물질

6

반응물 4

HCID 962WaterHCID 7477p-Anisoyl chlorideHCID 8471TriethylamineHCID 204805915-(1-Piperazinyl)-3,4-dihydrocarbostyril monohydrobromide

생성물 1

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

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매
2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b96a25f375e547de96f3ce2f53ef1fdd
출처 데이터셋
uspto-grants-1983_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04415572

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