참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Pentachlorophenol | HCID 992 | — |
| 반응물 | Dicyclohexylcarbodiimide | HCID 10868 | — |
| 반응물 | HCID 53248608 | HCID 53248608 | — |
| 촉매 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | HCID 53248609 | HCID 53248609 | 72.2% |
반응 단계
A solution of 10b (2.0 g, 6.4 mmol), pentachlorophenol (1.9 g, 7.0 mmol), DCC (1.6 g, 7.7 mmol) and DMAP (0.08 g, 0.64 mmol) in 100 mL of EtOAc was stirred at room temperature for 24 h. The mixture was filtered through celite and the solvent removed in vacuo. The crude product was purified by silica gel chromatography eluting with 25% EtOac-hexanes to give 2.6 g (72%) of 11b1 as white solid. 1H NMR (CDCl3, 300 MHz) δ 1.26-1.32 (m, 6H), 2.54 (d, J=1.2 Hz, 3H), 4.12-4.21 (m, 4H), 6.34 (d, J=1.2 Hz, 1H), 7.2 (d, J=8.7 Hz, 2H), 7.49 (d, J=8.7 Hz, 2H). 11C NMR (CDCl3, 75.0 MHz) δ 16.0, 16.1, 18.4, 64.8, 64.8, 68.9, 113.4, 120.2, 120.3, 128.0, 128.1, 131.2, 131.9, 137.8, 141.9, 144.3, 152.1, 160.6, 161.9. HRMS (M+H) calc, 560.9362; found, 560.9197.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08841257B2 |
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| 출처 데이터셋 | uspto-grants-2014_09 |
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| ORD ID | ord-45336e3cdda04410bbba6192b600804b |
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| 출처 메모 | uspto-grants-2014_09 |
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