Hydrochloric Acid → (S)-1-amino-3-methyl-4,5-dihydro-1H-benzo[d]azepin-2(3H)-one hydrochloride
反応式
C(O)(=O)[C@@H](C1C=CC=CC=1)O.[NH2:12][C@H:13]1[C:19]2[CH:20]=[CH:21][CH:22]=[CH:23][C:18]=2[CH2:17][CH2:16][N:15]([CH3:24])[C:14]1=[O:25].[ClH:26]>C(OCC)(=O)C>[ClH:26].[NH2:12][C@H:13]1[C:19]2[CH:20]=[CH:21][CH:22]=[CH:23][C:18]=2[CH2:17][CH2:16][N:15]([CH3:24])[C:14]1=[O:25]参加物
4
反応条件
- 温度
- 50 °C
実験手順
(S)-1-Amino-3-methyl-2,3,4,5-tetrahydro-1H-3-benzazepin-2-one (R)-mandelic acid salt (2.42 g, 7.06 mmol, 98.4% ee) was slurried in 25 mL ethyl acetate at ambient temperature. Concentrated aqueous hydrochloric acid (1.1 mL, about 11.2 mmol) was added and the mixture was heated to 50° C. with vigorous stirring for 3.5 hours. The slurry was cooled to ambient temperature and filtered, rinsed with the methyl t-butyl ether (about 10 mL) to give 1.48 g of the title compound (92.5% yield, 97.9% ee).