Ammonia → 6,7-Dihydro-2-methyl-1-(2-methylaminoethyl)-indolo[1,7-ab][1]benzazepine

Participants

Reaction Steps

For purification, the 6,7-dihydro-2-methyl-1-(2-methylaminoethyl)-indolo[1,7-ab][1]benzazepine was converted into the hydrochloride by dissolving in ethanol and treating with ethanolic hydrogen chloride. After a first crop of 28.6 g of the hydrochloride was obtained, the liquors no longer crystallised and were converted back into the base by shaking with an excess of ammonia and ether. The base was re-distilled and again treated with ethanolic hydrogen chloride to yield a second crop of 2 g of the hydrochloride. The two crops were combined and recrystallised from ethanol to give 27.9 g (38.4% yield) of 6,7-dihydro-2-methyl-1-(2-methylaminoethyl)-indolo[1,7-ab][1]benzazepine hydrochloride of melting point 210°-212° C. The pure hydrochloride was now suspended in water and shaken out with an excess of ammonia and ether to yield the pure base 6,7-dihydro-2-methyl-1-(2-methylaminoethyl)-indolo[1,7-ab][1]benzazepine as a pale-yellow viscous syrup of boiling point ca 160° C (air-bath temperature)/10- 5 mm Hg.

Provenance & Evidence