참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 4-Cyanophenylboronic acid | HCID 2734326 | — |
| 반응물 | Tert-butyl (6-bromopyridin-2-YL)carbamate | HCID 13040380 | — |
| 촉매 | HCID 178418397 | HCID 178418397 | — |
| 용매 | N,N-Dimethylformamide--water (1/1) | HCID 21962138 | — |
| 생성물 | [6-(4-Cyano-phenyl)-pyridin-2-yl]carbamic acid tert-butyl ester | HCID 67133691 | 60% |
반응 단계
A mixture of 4-cyanobenzeneboronic acid (7.35 g, 50 mmol), (6-bromo-pyridin-2-yl)carbamic acid tert-butyl ester (13.8 g, 50 mmol), Pd(Ph3P)4 (5.8 g, 0.15 mmol) and K2CO3 (10.4 g, 75 mmol) in DMF/H2O (1:1, 250 mL) was stirred under argon at 80° C. overnight. DMF was evaporated off under reduced pressure and the residue was dissolved in EtOAc (200 mL). The mixture was washed with water and brine, dried over Na2SO4, and concentrated to dryness. The residue was purified by column (Petroleum Ether/EtOAc 50:1) on silica gel to give [6-(4-cyano-phenyl)-pyridin-2-yl]carbamic acid tert-butyl ester (7.0 g, 60%). 1H NMR (300 MHz, CDCl3) δ 8.02-8.07 (m, 2H), 7.95 (d, J=8.4 Hz, 1H), 7.71-7.79 (m, 3H), 7.37-7.44 (m, 2H), 1.53 (s, 9H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08741933B2 |
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| 출처 데이터셋 | uspto-grants-2014_06 |
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| ORD ID | ord-fff1aa13543d4ff4b374fb4abf25f113 |
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| 출처 메모 | uspto-grants-2014_06 |
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