Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → {3-[3-(2-Fluoro-ethyl)-cyclobutyl]-phenylethynyl}-triisopropyl-silane
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | (Triisopropylsilyl)acetylene | HCID 2734682 | — |
| 반응물 | 1-Bromo-3-[3-(2-fluoro-ethyl)-cyclobutyl]-benzene | HCID 59305366 | — |
| 촉매 | Copper iodide | HCID 83717 | — |
| 촉매 | HCID 178418397 | HCID 178418397 | — |
| 생성물 | {3-[3-(2-Fluoro-ethyl)-cyclobutyl]-phenylethynyl}-triisopropyl-silane | HCID 59305330 | 80.4% |
반응 단계
In a CEM snap top microwave vial were combined 1-Bromo-3-[3-(2-fluoro-ethyl)-cyclobutyl]-benzene (0.250 gm 9.72 mmol), triisopropylsilylacetylene (0.22 gm, 1.21 mmol), copper iodide (7 mg, 0.178 mmol), tetrakis(triphenylphosphine)palladium (22 mg, 0.088 mmol) and triethylamine (0.600 g, 5.93 mmol). The vial was quickly agitated then irradiated in a CEM Explorer™ microwave instrument for 30 minutes at 80° C. Purification by column chromatography (hexanes) afforded an oil 349 mg. 1H NMR (400 MHz, DMSO-d6) δ ppm 1.06 (s, 21H) 1.62-1.81 (m, 2H) 1.82-1.97 (m, 1H) 2.00-2.45 (m, 4H) NMR (400 MHz, DMSO-d6) δ ppm 3.31-3.62 (m, 1H) 4.30-4.51 (m, 2H) 7.17-7.41 (m, 4H); MS (EI) m/z 256 [M+·].
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07723368B2 |
| 출처 데이터셋 | uspto-grants-2010_05 |
| ORD ID | ord-b3d943fd09aa4dbabfd02a842d180be4 |
| 출처 메모 | uspto-grants-2010_05 |