Benzenamine, 3-ethynyl- → HCID 16733971, Verbindung

HRID 2423007Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2423007
[Cl:1][C:2]1[C:11]2[C:6](=[CH:7][C:8]([O:16][C:17](=[O:19])[CH3:18])=[C:9]([O:12][C:13](=[O:15])[CH3:14])[CH:10]=2)[N:5]=[CH:4][N:3]=1.[C:20]([C:22]1[CH:23]=[C:24]([CH:26]=[CH:27][CH:28]=1)[NH2:25])#[CH:21]>>[ClH:1].[C:20]([C:22]1[CH:23]=[C:24]([NH:25][C:2]2[C:11]3[C:6](=[CH:7][C:8]([O:16][C:17](=[O:19])[CH3:18])=[C:9]([O:12][C:13](=[O:15])[CH3:14])[CH:10]=3)[N:5]=[CH:4][N:3]=2)[CH:26]=[CH:27][CH:28]=1)#[CH:21]

Komponenten

3

Edukt 2

HCID 104682Benzenamine, 3-ethynyl-HCID 272813776,7-Diacetoxy-4-chloro-quinazoline

Produkt 1

HCID 16733971HCID 16733971, VerbindungAusbeute 76,3 %

Reaktionsbedingungen

Temperatur
27.5 °C

Versuchsvorschrift

Into a 2.0 L four necked round-bottomed flask, equipped with a mechanical stirrer; reflux condenser and thermometer socket are charged the above organic layer containing 4-chloro-6,7-diacetoxy-quinazoline and 3-ethynylaniline (12 g). The reaction mass was slowly heated to reach reflux condition and maintained at reflux for 14 hours and the reaction was found to be over by HPLC. Then the reaction was cooled to 25-30° C. and filtered the mass, washed the cake with chloroform, and dried to get 29 g (76.3% by theory) of N-(3-ethynylphenyl)-6,7-diacetoxy-4-quinazolinamine hydrochloride as yellow solid.

Aufarbeitung

  1. temperaturereflux condenser
  2. additionthermometer socket are charged the above organic layer
  3. temperatureThe reaction mass was slowly heated
  4. temperatureto reach reflux condition
  5. temperaturemaintained
  6. temperatureat reflux for 14 hours
  7. filtrationfiltered the mass
  8. washwashed the cake with chloroform
  9. customdried

Quellen und Nachweise

ORD-Eintrag
ord-58a18d8468a549e8aa2c09c613a33f1c
Quelldatensatz
uspto-grants-2011_06
Patentnummer
US07960545B2

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