C=O.[C:3]([BH3-])#N.[Na+].Cl.[Cl:8][C:9]1[CH:10]=[CH:11][C:12]2[CH2:18][CH2:17][CH:16]([NH:19][CH3:20])[CH:15]=[CH:14][C:13]=2[CH:21]=1.C(O)(=O)C>C(#N)C>[Cl:8][C:9]1[CH:10]=[CH:11][C:12]2[CH2:18][CH2:17][CH:16]([N:19]([CH3:3])[CH3:20])[CH:15]=[CH:14][C:13]=2[CH:21]=17.7 ml of an aqueous solution of 40% formaldehyde and then 4.5 g of sodium cyanoborohydride were added to a mixture of 4.7 g of 2-chloro-7-methylamino-6,7-dihydro [5H] benzocycloheptene hydrochloride in 47 ml of acetonitrile and the mixture was stirred for 15 minutes at room temperature. Acetic acid was added to the reaction mixture until the pH was 7 and the mixture was stirred at room temperature for 45 minutes. The mixture was evaporated to dryness under reduced pressure to obtain 2.6 g of 2-chloro-7-dimethylamino-6,7-dihydro [5H] benzocycloheptene in the form of an oil. Addition of a solution of fumaric acid in methanol yielded 3.3 g of the fumarate of the said product melting at 160° C.
Loading…
