Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Carbon Dioxide → 5-Bromo-2,3-difluoro-4-(trimethylsilyl)benzoic acid
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Carbon Dioxide | HCID 280 | — |
| 반응물 | 2,2,6,6-Tetramethylpiperidine | HCID 13035 | — |
| 반응물 | (6-Bromo-2,3-difluorophenyl)trimethylsilane | HCID 23070109 | — |
| 반응물 | Butyllithium | HCID 178418339 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 5-Bromo-2,3-difluoro-4-(trimethylsilyl)benzoic acid | HCID 58538059 | — |
반응 단계
To a solution of n-BuLi (2.0 M in hexanes, 11.1 mL, 22.2 mmol) in anhydrous THF (17 mL) at −78° C. was added drop wise 2,2,6,6-tetramethylpiperidine (3.26 g, 22.1 mmol). After being stirred for 15 minutes, a solution of the product from step A (5.86 g, 22.1 mmol) in THF (20 mL) was added. The reaction mixture was stirred at −78° C. for 2 hours, then dry ice (100 g) was added. The mixture was allowed to stand at room temperature overnight, then it was diluted with water and extracted with EtOAc. The combined organics were dried over MgSO4, filtered, then concentrated to afford the title compound. The material was used directly in the next step without further purification. 1H NMR (500 MHz, CDCl3): δ 7.70 (d, J=4.4 Hz, 1H); 0.44 (s, 9H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08318667B2 |
| 출처 데이터셋 | uspto-grants-2012_11 |
| ORD ID | ord-a6c8e712035e4145a4b7fd1cc77e887a |
| 출처 메모 | uspto-grants-2012_11 |