反应详情

150 mg (0.38 mmol) of methyl 4-chloro-2-[1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridin-3-yl]pyrimidine-5-carboxylate (example 106A) and 78.5 mg (0.75 mmol) of formamidine hydrochloride were initially charged in 1.5 ml of DMF. Subsequently, 260 μl (1.89 mmol) of triethylamine were added and conversion was effected at 80° C. overnight. After cooling, the precipitated solid was filtered off and the mother liquor was then purified by means of preparative HPLC [column: Reprosil C18, 10 μm, 250*40 mm; eluent: acetonitrile/0.05% formic acid; gradient: 10% acetonitrile→>90% acetonitrile]. Thus, 65 mg (46% of theory) of the target compound were obtained.

1. temperatureAfter cooling
2. filtrationthe precipitated solid was filtered off
3. customthe mother liquor was then purified by means of preparative HPLC [column: Reprosil C18, 10 μm, 250*40 mm; eluent: acetonitrile/0.05% formic acid; gradient: 10% acetonitrile→>90% acetonitrile]
4. customThus, 65 mg (46% of theory) of the target compound were obtained