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

반응식

Cl.[CH3:2][C:3]1[C:19]2[C:6]3=[C:7]([CH:16]=[CH:17][CH:18]=2)[CH2:8][CH2:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[N:5]3[C:4]=1[CH2:20][CH2:21][NH:22][CH3:23].N.CCOCC>O>[CH3:2][C:3]1[C:19]2[C:6]3=[C:7]([CH:16]=[CH:17][CH:18]=2)[CH2:8][CH2:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[N:5]3[C:4]=1[CH2:20][CH2:21][NH:22][CH3:23]

참가 물질

실험 절차

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.