2-Chloro-6,7-dimethoxy-4-quinazolinamine → HCID 20473808, Verbindung

HRID 2295733Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2295733
[NH2:1][C:2]1[C:11]2[C:6](=[CH:7][C:8]([O:14][CH3:15])=[C:9]([O:12][CH3:13])[CH:10]=2)[N:5]=[C:4]([Cl:16])[N:3]=1.[C:17]([N:22]1[CH2:27][CH2:26][NH:25][CH2:24][CH2:23]1)(=[O:21])/[CH:18]=[CH:19]/[CH3:20]>C(O)CC(C)C>[OH2:12].[ClH:16].[NH2:1][C:2]1[C:11]2[C:6](=[CH:7][C:8]([O:14][CH3:15])=[C:9]([O:12][CH3:13])[CH:10]=2)[N:5]=[C:4]([N:25]2[CH2:26][CH2:27][N:22]([C:17](=[O:21])/[CH:18]=[CH:19]/[CH3:20])[CH2:23][CH2:24]2)[N:3]=1

Komponenten

4

Edukt 2

HCID 902352-Chloro-6,7-dimethoxy-4-quinazolinamineHCID 58756641-(Piperazin-1-yl)but-2-en-1-one

Produkt 1

HCID 20473808HCID 20473808, VerbindungAusbeute 90 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 31260Isoamyl AlcoholLösungsmittel

Versuchsvorschrift

To 80 ml of isopentanol were added 4.55 g of 4-amino-2-chloro-6,7-dimethoxyquinazoline and 3.4 g of 1-crotonoylpiperazine; the resulting mixture was then refluxed for 1.5 hours. At the end of this time, the hot reaction mixture was filtered. The filtrate was cooled and the crystals which resulted were collected by filtration and then recrystallized from ethanol to give 3.52 g of the desired hydrochloride hydrate of Compound No. 1 in the form of colourless crystals melting at 255°-256° C. (with decomposition):

Aufarbeitung

  1. temperaturethe resulting mixture was then refluxed for 1.5 hours
  2. filtrationAt the end of this time, the hot reaction mixture was filtered
  3. temperatureThe filtrate was cooled
  4. customthe crystals which resulted
  5. filtrationwere collected by filtration
  6. customrecrystallized from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-57021342419c40b6857ab907e9de6161
Quelldatensatz
uspto-grants-1984_01
Patentnummer
US04426382

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