Hydroxyamine hydrochloride → 6-{4-[3-(4-Chlorobenzoyl)-3-hydroxyliminopropyl]-1-piperazinylcarbonyl}-3,4-dihydrocarbostyril

HRID 477181노트

반응식

HRID 477181 반응식
ClC1C=CC(C([CH2:8][CH2:9][N:10]2[CH2:15][CH2:14][N:13]([C:16]([C:18]3[CH:19]=[C:20]4[C:25](=[CH:26][CH:27]=3)[NH:24][C:23](=[O:28])[CH2:22][CH2:21]4)=[O:17])[CH2:12][CH2:11]2)=O)=CC=1.[ClH:31].[NH2:32][OH:33].[C:34]([O-:37])(=O)[CH3:35].[Na+]>C(O)C.O>[Cl:31][C:18]1[CH:19]=[CH:20][C:25]([C:34]([C:35](=[N:32][OH:33])[CH2:8][CH2:9][N:10]2[CH2:11][CH2:12][N:13]([C:16]([C:18]3[CH:19]=[C:20]4[C:25](=[CH:26][CH:27]=3)[NH:24][C:23](=[O:28])[CH2:22][CH2:21]4)=[O:17])[CH2:14][CH2:15]2)=[O:37])=[CH:26][CH:27]=1

참가 물질

6

반응물 3

HCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 140997836-{4-[2-(4-Chlorobenzoyl)ethyl]-1-piperazinylcarbonyl}-3,4-dihydrocarbostyril

생성물 1

HCID 881243866-{4-[3-(4-Chlorobenzoyl)-3-hydroxyliminopropyl]-1-piperazinylcarbonyl}-3,4-dihydrocarbostyril

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

1.7 Grams of 6-{4-[2-(4-chlorobenzoyl)ethyl]-1-piperazinylcarbonyl}-3,4-dihydrocarbostyril, 0.83 g of hydroxylamine hydrochloride and 2.29 g of sodium acetate were dissolved in 40 ml of ethanol and 20 ml of water, and the solution was stirred overnight at room temperature. Then the reaction mixture was concentrated under reduced pressure, then the residue thus obtained was extracted with chloroform, the extract was dried with anhydrous sodium carbonate, then the solvent was removed by evaporation. The residue thus obtained was purified by means of a silica gel column chromatography (eluent: dichloromethane:methanol =50:1), then recrystallized from ethanol to yield 1.2 g of 6-{4-[3-(4-chlorobenzoyl)-3-hydroxyliminopropyl]-1-piperazinylcarbonyl}-3,4-dihydrocarbostyril.

후처리

  1. concentrationThen the reaction mixture was concentrated under reduced pressure
  2. customthe residue thus obtained
  3. extractionwas extracted with chloroform
  4. dry with materialthe extract was dried with anhydrous sodium carbonate
  5. customthe solvent was removed by evaporation
  6. customThe residue thus obtained
  7. customwas purified by means of a silica gel column chromatography (eluent: dichloromethane:methanol =50:1)
  8. customrecrystallized from ethanol

출처 및 근거

ORD 기록
ord-a509122c72404ccebe48d933b511434f
출처 데이터셋
uspto-grants-1989_12
특허 번호
US04886809

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