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Water → 6-[4-(2-Phenyl-2-hydroxyethyl)-1-piperazinylcarbonyl]-3,4-dihydrocarbostyril monohydrochloride

HRID 477180
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HRID 477180 반응식
C(C[CH2:10][N:11]1[CH2:16][CH2:15][N:14]([C:17]([C:19]2[CH:20]=[C:21]3[C:26](=[CH:27][CH:28]=2)[NH:25][C:24](=[O:29])[CH2:23][CH2:22]3)=[O:18])[CH2:13][CH2:12]1)(=O)C1C=CC=CC=1.[ClH:30].NO.[OH2:33]>N1C=CC=CC=1>[ClH:30].[C:19]1([CH:17]([OH:33])[CH2:10][N:11]2[CH2:16][CH2:15][N:14]([C:17]([C:19]3[CH:20]=[C:21]4[C:26](=[CH:27][CH:28]=3)[NH:25][C:24](=[O:29])[CH2:23][CH2:22]4)=[O:18])[CH2:13][CH2:12]2)[CH:20]=[CH:21][CH:26]=[CH:27][CH:28]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 443297Hydroxyamine hydrochlorideHCID 133698076-[4-(2-Benzoylethyl)-1-piperazinylcarbonyl]-3,4-dihydrocarbostyril

생성물 1

HCID 1317162096-[4-(2-Phenyl-2-hydroxyethyl)-1-piperazinylcarbonyl]-3,4-dihydrocarbostyril monohydrochloride

시약·촉매·용매 1

HCID 1049Pyridine용매

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온도
100 °C

실험 절차

20 Grams of 6-[4-(2-benzoylethyl)-1-piperazinylcarbonyl]-3,4-dihydrocarbostyril and 5.33 g of hydroxylamine hydrochloride were dispersed in 40 ml of pyridine and the suspension was stirred at 100° C. for 4 hours. After the reaction was completed, the reaction mixture was poured into water and then extracted with chloroform, the extract was dried with anhydrous potassium carbonate, then the solvent was removed by evaporation. The thus obtained residue was purified by means of a silica gel column chromatography (eluent: dichloromethane:methanol=50:1), then recrystallized from ethanol to yield 8.79 g of 6-[4-(3-hydroxyimino-3-phenylpropyl)-1-piperazinylcarbonyl]-3,4-dihydrocarbostyril 1/2-hydrate. White powdery substance.

후처리

  1. extractionextracted with chloroform
  2. dry with materialthe extract was dried with anhydrous potassium carbonate
  3. customthe solvent was removed by evaporation
  4. customThe thus obtained residue was purified by means of a silica gel column chromatography (eluent: dichloromethane:methanol=50:1)
  5. customrecrystallized from ethanol

출처 및 근거

ORD 기록
ord-5ccc7394814846f8a920133a453a62f7
출처 데이터셋
uspto-grants-1989_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04886809

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