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

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Reaction Steps

3 M hydrochloric acid prepared by diluting 36.2% concentrated hydrochloric acid (1.75 kg, 17.4 mol) with water (4.5 L) was added dropwise to an ethanol (123 L) suspension of 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 (3.53 kg, 7.74 mol) at a temperature from 21° C. to 22° C. over 30 minutes, while the suspension was stirred. The resulting mixture was stirred for 4 hours. The obtained crystal was collected by filtration, was then washed with ethanol (17.6 L), and was then dried under reduced pressure at 40° C. for 17 hours, so as to obtain the above title compound (3.50 kg, 7.2 mol). Yield: 93%.

Provenance & Evidence