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 (36 ml) and water (3.052 ml) were 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 (2.068 g, 4.485 mmol), and the resulting mixture was then stirred at 25° C. Thereafter, concentrated hydrochloric acid (0.045 ml, 0.54 mmol) was added to the reaction mixture over 1 minute, and the resulting mixture was then stirred for 9 minutes. This operation was repeated further nine times. Thereafter, the reaction mixture was stirred for 30 minutes, and concentrated hydrochloric acid (0.299 ml, 3.588 mmol) was added thereto. Then, ethanol (36 ml) was added thereto over 45 minutes, and the resulting mixture was then stirred for 4 hours. The precipitated crystal was filtrated, was then washed with ethanol (10 ml), and was then dried under reduced pressure at 40° C. for 30 minutes, so as to obtain the above title compound (2.020 g, 4.187 mmol). Yield: 93%.

Provenance & Evidence