Reacción #517675

ord-8cd17aacd98c4fd4b1e214110b25d3b0

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturacooling for 2 hours
  2. 2
    Otrothe solvents were removed at reduced pressure
  3. 3
    workup.ADDITIONThe residue was treated with water
  4. 4
    Otrothe resulting solid recrystallized from n-butanol

Procedimiento

A solution of 1.6 g of N-(3-bromophenyl)-4,6-quinazolindiamine in 15 ml of pyridine was cooled in an ice bath and a solution of 0.57 ml of trans-crotonoyl chloride in 6 ml of ether was added dropwise. After stirring and cooling for 2 hours, the solvents were removed at reduced pressure. The residue was treated with water and the resulting solid recrystallized from n-butanol to give 0.69 g of N-[4-[(3-bromophenyl)amino]-6-quinazolinyl]-(E)-2-butenamide: mp=153-160° C., mass spectrum (m/e): M+H 383, 385.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US06323209B1uspto-grants-2001_11