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 (51 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 23° C. Thereafter, 1.4 M hydrochloric acid (0.961 ml, 1.345 mmol) was added to the reaction mixture, and the resulting mixture was then stirred for 26 minutes. Then, 1.4 M hydrochloric acid (0.641 ml, 0.897 mmol) was added to the reaction mixture over 4 minutes, and the resulting mixture was then stirred for 6 minutes. This operation was repeated further three times. Thereafter, 1.4 M hydrochloric acid (0.320 ml, 0.448 mmol) was added to the reaction mixture, and the resulting mixture was then stirred for 30 minutes. Concentrated hydrochloric acid (0.299 ml, 3.588 mmol) was added to the reaction mixture, and the resulting mixture was then stirred for 1 hour. The reaction mixture was cooled to 2° C. over 50 minutes. Two hours 30 minutes 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