Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Trimethylsilylacetylene → 2-Chloro-1-ethynyl-4-(trifluoromethyl)benzene
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Trimethylsilylacetylene | HCID 66111 | — |
| 반응물 | Tetrabutylammonium Fluoride | HCID 2724141 | — |
| 반응물 | 3-Chloro-4-iodobenzotrifluoride | HCID 2736612 | — |
| 촉매 | Copper iodide | HCID 83717 | — |
| 촉매 | Dichlorobis(triphenylphosphine)palladium | HCID 6102075 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 2-Chloro-1-ethynyl-4-(trifluoromethyl)benzene | HCID 63668983 | 80.2% |
반응 단계
The title compound was prepared according to the procedure described in step-5 and step-6 of Intermediate-2 by using 2-chloro-1-iodo-4-(trifluoromethyl)benzene (1.0 g, 3.2 mmol), ethynyl(trimethyl)silane (0.541 g, 5.5 mmol), copper iodide (0.027 g, 0.14 mmol), bis(triphenylphosphine) palladium(II) chloride (0.050 g, 0.072 mmol), TBAF (catalytic) and DCM to afford 0.525 g of desired product. 1H NMR (300 MHz, DMSO d6): δ 4.88 (s, 1H), 7.73 (d, J=8.4 Hz, 1H), 7.83 (d, J=7.8 Hz, 1H), 8.01 (s, 1H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09439890B2 |
| 출처 데이터셋 | uspto-grants-2016_09 |
| ORD ID | ord-ffa5824dad7e47baabc1c01045922318 |
| 출처 메모 | uspto-grants-2016_09 |