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Hydrochloric Acid → 6-(3-Aminopropoxy)carbostyril

HRID 1856744
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1856744
C1(=O)[N:5]([CH2:6][CH2:7][CH2:8][O:9][C:10]2[CH:11]=[C:12]3[C:17](=[CH:18][CH:19]=2)[NH:16][C:15](=[O:20])[CH:14]=[CH:13]3)C(=O)C2=CC=CC=C12.O.NN.Cl>C(O)C>[NH2:5][CH2:6][CH2:7][CH2:8][O:9][C:10]1[CH:11]=[C:12]2[C:17](=[CH:18][CH:19]=1)[NH:16][C:15](=[O:20])[CH:14]=[CH:13]2
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 24654Hydrazine hydrate (1:1)HCID 117724126-(3-Phthalimidopropoxy)carbostyril

Produkt 1

HCID 100136326-(3-Aminopropoxy)carbostyrilAusbeute 74,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

To a suspension of 6-(3-phthalimidopropoxy)carbostyril (300 g) in ethanol (3 liters) is added hydrazine monohydrate (46 g), and the mixture is refluxed for 8 hours. After the mixture is allowed to cool, the precipitated crystals are collected by filtration, suspended in water, and the suspension thus obtained is acidified with conc. hydrochloric acid, and stirred for one hour. The insoluble materials are removed by filtration, and the filtrate is concentrated under reduced pressure to remove the solvent. The residue is neutralized to pH 7 with a 15% aqueous sodium hydroxide solution. The precipitated crystals are collected by filtration, and washed successively with ethanol and diethyl ether, and dried to give 6-(3-aminopropoxy)carbostyril (140 g) as a white powder.

Aufarbeitung

  1. temperaturethe mixture is refluxed for 8 hours
  2. temperatureto cool
  3. filtrationthe precipitated crystals are collected by filtration
  4. customthe suspension thus obtained
  5. customThe insoluble materials are removed by filtration
  6. concentrationthe filtrate is concentrated under reduced pressure
  7. customto remove the solvent
  8. filtrationThe precipitated crystals are collected by filtration
  9. washwashed successively with ethanol and diethyl ether
  10. customdried

Quellen und Nachweise

ORD-Eintrag
ord-e6fddc6f72094a0381cd978cdd7b4772
Quelldatensatz
uspto-grants-2000_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06143763

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