関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nilotinib Hydrochloride Anhydrous | HCID 16006490 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Nilotinib | HCID 644241 | — |
反応手順
36.0 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 a solvent mixture of 576 mL of methanol and 44.61 mL of water at 52° C. The solution is heated up to 64-66° C. in 15 minutes and kept for 5 minutes at 66° C. Then the solution is cooled down at 42° C. in minutes and the solution is seeded. The suspension is kept for 2.5 hours at 42° C., cooled down within 7 hours at 20° C., and maintained at this temperature for 11 hours. The methanol solvate form SC 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 is obtained.
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-5975855d81d74726ae7df87f40b55d86 |
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| 出典メモ | uspto-grants-2014_09 |
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