참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Methylamine hydrochloride | HCID 6364545 | — |
| 반응물 | N-(6-chloro-2-methylamino-pyrimidin-4-yl)-4-fluoro-benzenesulfonamide | HCID 19353544 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | N-(2,6-bis-methylamino-pyrimidin-4-yl)-4-fluoro-benzenesulfonamide | HCID 17774522 | 43.8% |
반응 단계
0.36 g (0.0011 mol) of N-(6-chloro-2-methylamino-pyrimidin-4-yl)-4-fluoro-benzenesulfonamide was dissolved in 10 ml of ethanol, treated with 1.2 g (0.018 mol) of methylamine hydrochloride and 4.0 ml (0.029 mol) of triethylamine and stirred in an autoclave at 140° C. for 17 hours. The mixture was freed completely from solvent, the residue was partitioned in ethyl acetate/water, the insoluble constituents were filtered off under suction and extracted. The extract and the solid were combined and recrystallized from methanol/diethyl ether. There was obtained 0.15 g (43%) of N-(2,6-bis-methylamino-pyrimidin-4-yl)-4-fluoro-benzenesulfonamide as white crystals; m.p. 261-263° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05998665 |
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| 출처 데이터셋 | uspto-grants-1999_12 |
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| ORD ID | ord-3902cd16a7da44ad949b8b757e1ce5a1 |
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| 출처 메모 | uspto-grants-1999_12 |
|---|