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 (41 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, 1.8 M hydrochloric acid (0.748 ml, 1.346 mmol) was added to the reaction mixture, and the resulting mixture was then stirred for 27 minutes. Then, 1.8 M hydrochloric acid (0.498 ml, 0.896 mmol) was added to the reaction mixture over 5 minutes, and the resulting mixture was then stirred for 5 minutes. This operation was repeated further three times. 1.8 M hydrochloric acid (0.249 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 3° C. over 50 minutes. Two hours 20 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 (2.070 g, 4.291 mmol). Yield: 96%.

Provenance & Evidence