Ethanol → HCID 67916296, compound

Participants

Reaction Conditions

Reaction Steps

18 g, approximately 0.05 moles of 3-carbisopropoxyamino-5-chloroacetyl-10,11-dihydro-5H-dibenz[b,f]azepine (hereafter referred to as Startazeine 2) and 300 ml of 96% ethanol are added to a 2liter 3-neck flask. At room temperature, 100 ml of aqueous monomethylamine solution (38%=1.2 moles) are added with stirring. The reaction mixture is heated slowly by means of a water bath to 50° C., stirred for 3 hours at this temperature and then for another hour at 60° C. After cooling to 25° C.-30° C., 750 ml of cold water are added. After standing overnight, an additional 400 ml of water are added with stirring. The water-amine-alcohol mixture is decanted from the oily deposit formed and same amount of fresh water is added. After decanting the supernatant once more, the oily residue is dissolved in 80 ml of warm acetone, cleaned through a filter and induced to crystallize in the refrigerator. The yield is 11 g, or 60% of the theoretical yield. The melting point is 150° C.-152° C. The empirical formula is C21H25N3O3, and the molecular weight is 367.46.

Provenance & Evidence