참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methanol | HCID 887 | — |
| 반응물 | Imatinib | HCID 5291 | — |
| 반응물 | Dichloromethane | HCID 6344 | — |
| 반응물 | Methanesulfonic Acid | HCID 6395 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | Imatinib Mesylate | HCID 123596 | — |
반응 단계
Imatinib free base (90 g), methanol (450 mL) and dichloromethane (270 mL) were stirred at 25° C. in round bottom flask in presence of nitrogen. Methanesulfonic acid (18 g) was slowly added to the reaction mixture at 25° C. Water (27 mL) was added and the reaction mixture was stirred for 2 hours. The reaction mixture was heated at 50° C. and concentrated to remove the solvent mixture. The residue was degassed at 60° C. and cooled to 25° C. Methyl tert-butyl ether (630 mL) was added to the reaction mixture and stirred for 45 minutes. The product was filtered and washed with methyl tert-butyl ether. The product was dried at 60° C. under high vacuum for 10 hours to obtain amorphous imatinib mesylate. Water content 0.90%.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09439903B2 |
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| 출처 데이터셋 | uspto-grants-2016_09 |
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| ORD ID | ord-af1762d853804d258e309783c217d2cb |
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| 출처 메모 | uspto-grants-2016_09 |
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