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HRID 72809作成日:2026年10月25日

Water → Nilotinib

https://huagongshe.com/reaction/72809

反応式

関与物質

役割名称HCID仕込み量
反応物WaterHCID 962—
反応物Nilotinib Hydrochloride AnhydrousHCID 16006490—
溶媒MethanolHCID 887—
生成物NilotinibHCID 644241—

反応条件

温度65 °C

反応手順

12 g 4-methyl-N-[3-(4-methyl-imidazol-1-yl)-5-trifluoromethyl-phenyl]-3-(4-pyridin-3-yl-pyrimidin-2-ylamino)-benzamide hydrochloride is dissolved in 192 mL of methanol and 21 ml of water at 52° C. The solution is heated to 64-66° C. in 10 minutes and let stand for 45 minutes. The solution is then cooled down in 3 hours at 0° C. The solution spontaneously crystallized before 0° C.; therefore, the cooling ramp was stopped at 20° C. and let stand with stirring for 2 days. The suspension is cooled down to 0° C. in 2 hours before filtration under vacuum to obtain form A of the hydrochloride salt of 4-methyl-N-[3-(4-methyl-imidazol-1-yl)-5-trifluoromethyl-phenyl]-3-(4-pyridin-3-yl-pyrimidin-2-ylamino)-benzamide.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08829015B2
出典データセットuspto-grants-2014_09
ORD IDord-92fa8f28f2d24bde94debe8af8480d31
出典メモuspto-grants-2014_09