참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methanesulfonic Acid | HCID 6395 | — |
| 반응물 | HCID 178488203 | HCID 178488203 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | HCID 178488204 | HCID 178488204 | 108.2% |
반응 단계
A warmed solution of trans-N2-(4-{4-amino-1-[4-(4-methylpiperazino)cyclohexyl]-1H-pyrazolo[3,4-d]pyrimidin-3-yl}-2-methoxyphenyl)-1-methyl-1H-2-indolecarboxamide (0.072 g, 0.12 mmol) in ethyl acetate (20 mL) was treated with methane sulfonic acid (0.012 g, 0.12 mmol). A precipitate slowly formed and was filtered under a nitrogen atmosphere to give 0.051 g of trans-N2-(4-{4-amino-1-[4-(4-methylpiperazino)cyclohexyl]-1H-pyrazolo[3,4-d]pyrimidin-3-yl}-2-methoxyphenyl)-1-methyl-1H-2-indolecarboxamide di-mesylate. The melting range was determined to be 345.5 to 348.1° C. 1H NMR (d6-DMSO) δ 9.4353 (s, 1H), 8.2461 (s, 1H), 8.1239-8.1035 (d, 1H, J=8.16 Hz), 7.7182-7.6985 (d, 1H, J=7.88 Hz), 7.6004-7.5792 (d, 1H, J=8.48 Hz), 7.3442-7.2794 (m, 4H), 7.1718-7.1349 (t, 1H), 4.6829 (m, 1H), 4.0396 (s, 3H), 3.9570 (s, 3H), 2.6703 (m, 6H), 2.5 (s, 3H), 2.2949 (s, 6H), 2.0891-2.9086 (m, 7H), 1.5179 (m, 2H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06921763B2 |
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| 출처 데이터셋 | uspto-grants-2005_07 |
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| ORD ID | ord-0b59c27ab57a485f979e5f4bb4b6f361 |
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| 출처 메모 | uspto-grants-2005_07 |
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