Hydrochloric Acid → 5-[2-Hydroxy-3-(4-phenylpiperazinyl)propoxy]-3,4-dihydro carbostyril monohydrochloride

HRID 569955노트

반응식

HRID 569955 반응식
[O:1]1[CH2:16][CH:2]1[CH2:3][O:4][C:5]1[CH:14]=[CH:13][CH:12]=[C:11]2[C:6]=1[CH2:7][CH2:8][C:9](=[O:15])[NH:10]2.[C:17]1([N:23]2[CH2:28][CH2:27][NH:26][CH2:25][CH2:24]2)[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.[ClH:29].C(O)C>CO.CC(C)=O>[ClH:29].[OH:1][CH:2]([CH2:16][N:26]1[CH2:27][CH2:28][N:23]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH2:24][CH2:25]1)[CH2:3][O:4][C:5]1[CH:14]=[CH:13][CH:12]=[C:11]2[C:6]=1[CH2:7][CH2:8][C:9](=[O:15])[NH:10]2

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 70961-PhenylpiperazineHCID 128994235-[(Oxiran-2-yl)methoxy]-3,4-dihydroquinolin-2(1H)-one

생성물 1

HCID 128994275-[2-Hydroxy-3-(4-phenylpiperazinyl)propoxy]-3,4-dihydro carbostyril monohydrochloride

시약·촉매·용매 2

HCID 180Acetone용매HCID 887Methanol용매

실험 절차

4.4 Grams of 5-(2,3-epoxypropoxy)-3,4-dihydrocarbostyril and 3.4 g of 4-phenylpiperazine are dispersed in 60 ml of methanol and reacted at 50°-60° C. for 3 hours. After the reaction is completed, the reaction mixture is concentrated under a reduced pressure. To the residue thus obtained are added 5 ml of concentrated hydrochloric acid and 30 ml of ethanol to dissolve the residue uniformly and further 200 ml of acetone are added. The crystals precipitated are collected by filtration and dried. Recrystallization from water obtains 6.5 g of 5-[2-hydroxy-3-(4-phenylpiperazinyl)propoxy]-3,4-dihydrocarbostyril monohydrochloride in the form of colorless needle-like crystals with a melting point of 239°-241° C.

후처리

  1. customreacted at 50°-60° C. for 3 hours
  2. concentrationthe reaction mixture is concentrated under a reduced pressure
  3. customTo the residue thus obtained
  4. dissolutionto dissolve the residue uniformly
  5. customThe crystals precipitated
  6. filtrationare collected by filtration
  7. customdried
  8. customRecrystallization from water

출처 및 근거

ORD 기록
ord-f448c440e4f4405484860cae6cb7d71e
출처 데이터셋
uspto-grants-1988_03
특허 번호
US04734416

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