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

HRID 621555Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 621555
[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

Komponenten

7

Edukt 4

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

Produkt 1

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

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 180AcetoneLösungsmittelHCID 887MethanolLösungsmittel

Versuchsvorschrift

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 to obtain 6.5 g of 5-[2-hydroxy-3-(4-phenylpiperazinyl)propoxy]-3,4-dihydro carbostyril monohydrochloride in the form of colorless needle-like crystals with a melting point of 239°-241° C.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-991eddb2af6c4c9aad9ac27f672eeaa6
Quelldatensatz
uspto-grants-1989_04
Patentnummer
US04824840

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