Hydrochloric Acid → HCID 68735414, compound

Participants

Reaction Steps

To a solution of 0.040 g (0.09 mmol) of (+/−)-4-chloro-2-methoxy-N-(4-oxo-2-pyrimidin-4-yl-4,5,6,7,8,9-hexahydro-1,4a,7-triaza-benzocyclohepten-9-yl)-benzamide in 1.9 ml of methanol was added 0.003 g (0.04 mmol) of paraformaldehyde, 0.022 g (0.10 mmol) of sodium triacetoxyborohydride and 40 μL (0.20 mmol) of hydrochloric acid (5-6N in isopropanol). The reaction mixture was stirred at room temperature for 12 hours. To the resulting mixture was added 0.006 g (0.07 mmol) of paraformaldehyde 0.042 g (0.20 mmol) of sodium triacetoxyborohydride and pH was adjusted to 6 with glacial acetic acid. The resulting mixture was stirred at room temperature for 2 hours. The reaction mixture was concentrated; the residue was dissolved in dichloromethane, washed with a saturated aqueous solution of sodium carbonate, saturated aqueous solution of sodium chloride, dried over sodium sulfate and evaporated. The free base was transformed into its hydrochloride salt to give 0.035 g of pure product.

Provenance & Evidence