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 (36.7 L) 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 (1.07 kg, 2.28 mol), and the resulting mixture was then stirred at 24° C. Thereafter, 1 M hydrochloric acid (2.06 L, 2.06 mol) was added to the reaction mixture over 68 minutes. Then, concentrated hydrochloric acid (57 ml, 0.68 mol) was further added to the reaction mixture over 34 minutes, and the resulting mixture was then stirred for 30 minutes. Thereafter, concentrated hydrochloric acid (191 ml, 2.29 mol) was added to the reaction mixture over 9 minutes, and the resulting mixture was then stirred for 1 hour. The reaction mixture was cooled to 5° C. over 76 minutes. Twenty-two hours 30 minutes later, the precipitated crystal was filtrated, was then washed with ethanol (5 L), and was then dried under reduced pressure at 40° C. for 18 hours, so as to obtain the above title compound (1.05 kg, 2.18 mol). Yield: 95%.

Provenance & Evidence