Reacción #4930

ord-899dfc4eb3d343fca6a7503b6a131990

Ecuación de reacción

CNC
dimethylamine
CN1CC(CCCl)Sc2ncccc2C1=O
2-(2-chloroethyl)-2,3-dihydro-4-methylpyrido[3,2-f][1,4]-thiazepin-5(4H)-one
CNC
dimethylamine
CN(C)CCC1CN(C)C(=O)c2cccnc2S1.Cl.Cl
2-[2-(Dimethylamino)ethyl]-2,3-dihydro-4-methylpyrido[3,2-f][1,4]-thiazepin-5(4H)-one dihydrochloride

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Otroto evaporate
  2. 2
    Otrothe residue was partitioned between chloroform and dilute sodium hydroxide
  3. 3
    ConcentraciónThe chloroform layer was concentrated
  4. 4
    workup.DISSOLUTIONthe residue, the free base of the title compound, was dissolved in isopropyl alcohol
  5. 5
    Otroreacted with hydrogen chloride

Procedimiento

A solution of 1.5 g (0.0058 mole) of 2-(2-chloroethyl)-2,3-dihydro-4-methylpyrido[3,2-f][1,4]-thiazepin-5(4H)-one in 20 ml of dimethylamine was stirred at 25° C. in a sealed container for 72 hr. The excess dimethylamine was allowed to evaporate and the residue was partitioned between chloroform and dilute sodium hydroxide. The chloroform layer was concentrated and the residue, the free base of the title compound, was dissolved in isopropyl alcohol and reacted with hydrogen chloride. The resulting hydrochloride salt weighted 1.5 g (77%), m.p.>250° C.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04727152uspto-grants-1988_02