関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Isopropanol | HCID 3776 | — |
| 反応物 | Imatinib | HCID 5291 | — |
| 反応物 | Methanesulfonic Acid | HCID 6395 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Imatinib Mesylate | HCID 123596 | — |
反応手順
Methanesulfonic acid (ca. 0.99 eq.) was added, with stirring to a suspension of Imatinib (10.647 g) in ethyl alcohol (173 mL) heated previously to 65° C. and the mixture was stirred for 5 min. The seeds of the α-crystal form (0.279 g) were added to the solution at approx. 44° C. followed by dropwise addition of isopropyl alcohol (65 mL) and ethyl acetate (238 mL). Stirring at room temperature (approx. 24-25° C.) was continued for 4 hours and then the mixture was left without stirring for 64 h. The product was filtered off and washed with 50 mL of ethyl acetate. The crystals were dried under reduced pressure at room temperature to afford 11.85 g (93.1%) of α-crystal form of Imatinib monomesylate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07732601B2 |
|---|
| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-8b07da66c7b84ae4b6c6d39409d2fcd6 |
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| 出典メモ | uspto-grants-2010_06 |
|---|