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

HRID 1460680노트

반응식

HRID 1460680 반응식
ClC1C=CC(C(CC[C:10]2([C:21]([N:23]3[CH2:28][CH2:27][NH:26][CH2:25][CH2:24]3)=[O:22])[CH2:19][C:18]3[C:13](=[CH:14][CH:15]=C[CH:17]=3)[NH:12]C2=O)=O)=CC=1.[ClH:31].[NH2:32][OH:33].[C:34]([O-:37])(=O)[CH3:35].[Na+].[CH2:39]([OH:41])[CH3:40]>O>[Cl:31][C:13]1[CH:18]=[CH:17][C:40]([C:39]([C:19](=[N:32][OH:33])[CH2:10][CH2:21][N:26]2[CH2:25][CH2:24][N:23]([C:21]([C:10]3[CH:19]=[C:18]4[C:13](=[CH:14][CH:15]=3)[NH:12][C:34](=[O:37])[CH2:35][CH2:17]4)=[O:22])[CH2:28][CH2:27]2)=[O:41])=[CH:15][CH:14]=1

참가 물질

6

반응물 4

HCID 702EthanolHCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 1317170952-(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 1

HCID 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. White powdery substance. Melting point: 207° C.-209° C. (decomp.).

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-8cf757d0714b4a5aa2e8e9b21c6197bc
출처 데이터셋
uspto-grants-1991_12
특허 번호
US05071856

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