참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetic Anhydride | HCID 7918 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 4-{3E-[5-(1H-indol-2-yl)-2,4-dimethoxyphenyl]acryloyl}benzenesulfonamide | HCID 21041627 | — |
| 촉매 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | HCID 11191334 | HCID 11191334 | 62% |
반응 단계
To a solution of 4-{3E-[5-(1H-indol-2-yl)-2,4-dimethoxyphenyl]acryloyl}benzenesulfonamide (Ex-35E, 0.462 g, 1 mmol), DMAP (0.012 g, 0.1 mmol), and Et3N (0.1 g, 1.05 mmol) in 50 ml of THF, was added Ac2O (0.204 g, 2 mmol). The reaction mixture was stirred at room temperature overnight. The yellow solid precipitated was filtered and redissolved in 50% ethanol in water (50 mL). The clear solution was then adjusted to pH1, and the solid formed was filtered and washed with water to give 0.31 g (62%) the title compound as a red solid, mp 218–220° C. 1H-NMR (300 MHz, DMSO-d6) δ 12.26 (br, 1H), 11.15 (s, 1H), 8.32 (s, 1H), 8.25 (d, J=8 Hz, 2H), 8.04–8.09 (m, 3H), 7.83 (d, J=15 Hz, 1H), 7.49 (d, J=7 Hz, 1H), 7.42 (d, J=8 Hz, 1H), 7.02–7.07 (m, 1H), 6.93–6.97(m, 2H), 6.82 (s, 1H), 4.03 (s, 3H), 3.99 (s, 3H), 1.94 (s, 3H). HRMS (EI) Calcd for C27H24N2O6S: 504.1335 ([M]+); Found: 504.1365.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07173129B2 |
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| 출처 데이터셋 | uspto-grants-2007_02 |
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| ORD ID | ord-75bf753cebcb4f7b8644527da72b4611 |
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| 출처 메모 | uspto-grants-2007_02 |
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