Reacción #63449

ord-62a3a9f5b00e4b3493aa4800d32f3db5

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Extracciónthe whole is extracted with methylene chloride
  2. 2
    LavadoThe combined extracts are washed with 10% sodium carbonate solution
  3. 3
    Secadodried over anhydrous sodium sulphate
  4. 4
    Otroevaporated under reduced pressure

Procedimiento

1.19 g of 5,7-dihydro-6H-dibenz[c,e]azepine-6-carboxamide are dissolved in 10 ml of methylene chloride, and the solution is treated with 1.14 g of triethyloxonium tetrafluoroborate and stirred at room temperature for 20 hours. The mixture is then poured on to 10% sodium carbonate solution/ice and the whole is extracted with methylene chloride. The combined extracts are washed with 10% sodium carbonate solution, dried over anhydrous sodium sulphate and evaporated under reduced pressure. In this manner there is obtained crude ethyl 5,7-dihydro-6H-dibenz[c,e]azepine-6-caboximidate which is purified by a filtration on silica gel [eluent: n-hexane/ethyl acetate (1:1)]; m.p. 74°-76° C. (crystallized from n-hexane).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04766115uspto-grants-1988_08