Reacción #738429

ord-d510fa2bebd14e89b7752766e94a7a14

Disolventes

Condiciones de reacción

Temperatura
80°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    workup.DISTILLATIONExcess 2-chloroacrylonitrile is distilled off in vacuo
  2. 2
    Filtraciónthe precipitated product is filtered off
  3. 3
    Lavadowashed with water
  4. 4
    Otrodried
  5. 5
    Otro(yield 1.1 g; 87% of theory), m.p. 214-216° C. (recrystallization from ethyl acetate/toluene)

Procedimiento

A mixture of 3-azido-2,3,4,5-tetrahydro-2-oxo-1H-1-benzazepine (1.01 g) and 2-chloroacrylonitrile (0.95 g) in water (5 ml) is stirred at about 80° C. for 18 hours. Excess 2-chloroacrylonitrile is distilled off in vacuo, and the precipitated product is filtered off, washed with water and dried (yield 1.1 g; 87% of theory), m.p. 214-216° C. (recrystallization from ethyl acetate/toluene).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US06277999B1uspto-grants-2001_08