Reacción #84652

ord-69a23d5d36bf4cc69ee11cb718be1394

Disolventes

Condiciones de reacción

Temperatura
70°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Otrowas degassed with N2 for 5 mins
  2. 2
    TemperaturaThe mixture was cooled to room temperature
  3. 3
    Concentraciónconcentrated
  4. 4
    Otrothe residue was purified by silica gel column chromatography

Procedimiento

A mixture of 2-chloro-6-(2,6-dichloro-3,5-dimethoxyphenyl)quinazoline (0.95 g, 2.6 mmol), tert-butyl ((1S,2R)-2-aminocyclohexyl)carbamate (1.1 g, 5.14 mmol), and DBU (0.77 mL, 5.14 mmol) in acetonitrile (9 mL) was degassed with N2 for 5 mins and heated at 70° C. for 16 h. The mixture was cooled to room temperature, concentrated and the residue was purified by silica gel column chromatography to afford tert-butyl ((1S,2R)-2-((6-(2,6-dichloro-3,5-dimethoxyphenyl)quinazolin-2-yl)amino)cyclohexyl)carbamate (1.1 g, 81%). MS (ES+) C27H32Cl2N4O4 requires: 546, found: 547 [M+H]+.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US09434700B2uspto-grants-2016_09