Reacción #4926

Ecuación de reacción

2-(2-chloroethyl)-2,3-dihydro-4-methylpyrido[4,3-f][1,4]-oxazepine-5(4H)-thione

dimethylamine

→

2-[2-(Dimethylamino)ethyl]-2,3-dihydro-4-methylpyrido[4,3-f][1,4]-oxazepine-5(4H)-thione hydrochloride

Disolventes

ethyl alcohol

Condiciones de reacción

Tratamiento posterior

1. 1
   FiltraciónThe resulting solution was filtered
2. 2
   Concentraciónconcentrated
3. 3
   workup.DISSOLUTIONThe residue was dissolved in isopropyl alcohol
4. 4
   workup.ADDITIONa few drops of ethereal hydrogen chloride were added
5. 5
   OtroThe hydrochloride salt crystals were recrystallized
6. 6
   workup.DISSOLUTIONby dissolving in ethyl alcohol
7. 7
   Otroabove 200° C.

Procedimiento

To a solution of 0.5 g (0.002 mole) of 2-(2-chloroethyl)-2,3-dihydro-4-methylpyrido[4,3-f][1,4]-oxazepine-5(4H)-thione in 20 ml of ethyl alcohol was added 2 ml of 40% aqueous dimethylamine. The mixture was heated in a steel bomb to 100° C. for 14 hr. The resulting solution was filtered and concentrated. The residue was dissolved in isopropyl alcohol and a few drops of ethereal hydrogen chloride were added. The hydrochloride salt crystals were recrystallized by dissolving in ethyl alcohol and boiling while replacing the ethyl alcohol with isopropyl alcohol. The yield of product was 0.3 g (47%), m.p.: decomp. above 200° C.

Fuente