Hydrochloric Acid → 2-{4-Amino-2-[(3-chloro-4-methoxy-5-methylpyridin-2-yl)methyl]-2,7-dihydro-6-thia-1,2,3,5-tetraazabenzo[cd]azulen-8-yl}-N-methylacetamide hydrochloride

Participants

Reaction Conditions

Reaction Steps

Ethanol (180 ml) was added to 2-{4-amino-2-[(3-chloro-4-methoxy-5-methylpyridin-2-yl)methyl]-2,7-dihydro-6-thia-1,2,3,5-tetraazabenzo[cd]azulen-8-yl}-N-methylacetamide (5.252 g, 11.21 mmol), and the resulting mixture was then stirred at 26° C. Thereafter, 1 M hydrochloric acid (10.09 ml, 10.09 mmol) was added to the reaction mixture over 1 hour. Then, concentrated hydrochloric acid (0.280 ml, 3.360 mmol) was further added to the reaction mixture over 30 minutes, and the resulting mixture was then stirred for 30 minutes. Thereafter, concentrated hydrochloric acid (0.934 ml, 11.21 mmol) was added to the reaction mixture over 7 minutes, and the resulting mixture was then stirred for 1 hour. The reaction mixture was cooled to 5° C. over 1 hour. Twenty hours later, the precipitated crystal was filtrated, was then washed with ethanol (25 ml), and was then dried under reduced pressure at 40° C. for 1 hour, so as to obtain the above title compound (5.145 g, 10.67 mmol). Yield: 95%.

Provenance & Evidence