関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Nilotinib Hydrochloride Anhydrous | HCID 16006490 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Nilotinib | HCID 644241 | — |
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
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08829015B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-92fa8f28f2d24bde94debe8af8480d31 |
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| 出典メモ | uspto-grants-2014_09 |
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