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Hydrochloric Acid → 5H-Pyrido(2,3-b)(1,5)benzodiazepin-5-one, 6,11-dihydro-11-methyl-

HRID 1898870
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1898870
C([N:9]1[C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=2[N:13]([CH3:20])[C:12]2[N:21]=[CH:22][CH:23]=[CH:24][C:11]=2[C:10]1=[O:25])(=O)C1C=CC=CC=1.Cl>C(O)C>[CH3:20][N:13]1[C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=2[NH:9][C:10](=[O:25])[C:11]2[CH:24]=[CH:23][CH:22]=[N:21][C:12]1=2
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 23372616HCID 23372616, Verbindung

Produkt 1

HCID 4532425H-Pyrido(2,3-b)(1,5)benzodiazepin-5-one, 6,11-dihydro-11-methyl-

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A mixture of 9.4 g (0.0285 mol) of the product obtained in step b, 150 ml ethanol and 5 ml concentrated aqueous hydrochloric acid was refluxed for five hours while stirring. The clear yellowish solution that had been formed was set aside overnight. The resulting precipitate was collected by filtration and thoroughly washed with diluted aqueous ammonia. The product was dried overnight in a stream of nitrogen at room temperature and thereafter was recrystallized from n-propanol. The colorless product had a m.p. of 235°-237° C. and was identified as 6,11-dihydro-11-methyl-5H-pyrido-[2,3-b][1,5]benzodiazepin-5-one. The yield was 3.3 g (51% of theory).

Aufarbeitung

  1. temperaturewas refluxed for five hours
  2. customThe clear yellowish solution that had been formed
  3. filtrationThe resulting precipitate was collected by filtration
  4. washthoroughly washed with diluted aqueous ammonia
  5. customThe product was dried overnight in a stream of nitrogen at room temperature
  6. customwas recrystallized from n-propanol

Quellen und Nachweise

ORD-Eintrag
ord-4c31e871222f4032a54af35a52ccfe0d
Quelldatensatz
uspto-grants-1996_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05571809

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