Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Pinacol → 5-(1,3-Dioxolan-2-yl)-2-fluoro-3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Pinacol | HCID 6425 | — |
| 반응물 | Sulfuric acid magnesium salt (1:1) | HCID 24083 | — |
| 반응물 | 5-(1,3-Dioxolan-2-yl)-2-fluoropyridin-3-ylboronic acid | HCID 59548367 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 5-(1,3-Dioxolan-2-yl)-2-fluoro-3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridine | HCID 59548432 | 95.1% |
반응 단계
5-(1,3-Dioxolan-2-yl)-2-fluoropyridin-3-ylboronic acid (14.56 g, 68.4 mmol) was suspended in PhMe (300 mL) and anhydrous magnesium sulfate (41.223 g, 342 mmol) and pinacol (8.27 g, 70.0 mmol) were added. The reaction was stirred under nitrogen at room temperature over the weekend. The suspension was filtered, and the solid was washed with EtOAc. The filtrate was washed with brine (2×200 mL), and the organic phase was dried over sodium sulfate, filtered, concentrated and dried to give 19.19 g of 5-(1,3-dioxolan-2-yl)-2-fluoro-3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridine as a light yellow powder. 1H NMR (CDCl3, 400 MHz) δ 8.39 (d, J=2.54 Hz, 1H); 8.28 (dd, J=8.02 Hz, 2.54 Hz, 1H); 5.84 (s, 1H); 4.17-4.04 (m, 4H); 1.37 (s, 12H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08362241B2 |
| 출처 데이터셋 | uspto-grants-2013_01 |
| ORD ID | ord-5fb35fa314594e28841d51184b9be16e |
| 출처 메모 | uspto-grants-2013_01 |