Reacción #78819

ord-45b050ef2cc34fdbb9b9b60df9738e49

Condiciones de reacción

Temperatura
170°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    OtroThe warm reaction mixture
  2. 2
    Otrothe hydrochloride salt, which is crystallizing
  3. 3
    Temperaturaon cooling
  4. 4
    Filtraciónis filtered off

Procedimiento

A solution of 2-chloro-4-phenylamino-quinazoline (0.92 g) (prepared as described in Example 1a and N-methyl-(4-aminophenyl)-methanesulfonamide (0.80 g) in 10 ml of isopentylalcohol is stirred under nitrogen at 170° C. for 15 min in a sealed vessel. The warm reaction mixture is diluted with 10 ml ethanol and the hydrochloride salt, which is crystallizing on cooling, is filtered off to yield N-methyl-[4-(4-phenylamino-quinazolin-2-ylamino)-phenyl]-methanesulfonamide hydrochloride as light yellow crystals melting at 259-263° C.; Rf (A2) 0.11, FAB-MS: (M+H)+=420. Analytical data: C22H21N5O2S+HCl.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US06713265B1uspto-grants-2004_03