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 (72 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 (2.068 g, 4.485 mmol), and the resulting mixture was then stirred at 26° C. Thereafter, 1 M hydrochloric acid (4.037 ml, 4.037 mmol) was added to the reaction mixture over 1 hour. Then, concentrated hydrochloric acid (0.111 ml, 1.332 mmol) was further added to the reaction mixture over 5 minutes, and the resulting mixture was then stirred for 30 minutes. Thereafter, concentrated hydrochloric acid (0.374 ml, 4.488 mmol) was added to the reaction mixture over 6 minutes, and the resulting mixture was then stirred for 1 hour. The reaction mixture was cooled to 5° C. over 1 hour. Two hours later, 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 (2.042 g, 4.233 mmol). Yield: 94%.

Provenance & Evidence