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 24° C. Thereafter, 1 M hydrochloric acid (1.346 ml, 1.346 mmol) was added to the reaction mixture, and the resulting mixture was then stirred for 25 minutes. Then, 1 M hydrochloric acid (0.897 ml, 0.897 mmol) was added to the reaction mixture over 4 minutes, and the resulting mixture was then stirred for 7 minutes. This operation was repeated further twice. Thereafter, concentrated hydrochloric acid (0.037 ml, 0.444 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 twice, and the reaction mixture was then stirred for 30 minutes. Concentrated hydrochloric acid (0.374 ml, 4.488 mmol) was added to the reaction mixture, and the resulting mixture was then stirred for 1 hour. The reaction mixture was cooled to 10° 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 (2.048 g, 4.246 mmol). Yield: 95%.

Provenance & Evidence