Reaktion #4926

Reaktionsgleichung

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

Lösungsmittel

ethyl alcohol

Reaktionsbedingungen

Aufarbeitung

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

Vorschrift

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.

Quelle