Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dimethylformamide → (4-Bromophenylethynyl)trimethylsilane
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 1-Bromo-2-iodobenzene | HCID 11415 | — |
| 반응물 | Trimethylsilylacetylene | HCID 66111 | — |
| 촉매 | Copper iodide | HCID 83717 | — |
| 촉매 | HCID 178418476 | HCID 178418476 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | (4-Bromophenylethynyl)trimethylsilane | HCID 4226980 | 105.9% |
반응 단계
A mixture of 150 g of 97% bromo iodo benzene, 500 ml of anhydrous dimethylformamide, 100 ml of triethylamine, 50 g of trimethylsilyl acetylene, 2.1 g of copper iodide and 2.22 g of bis-(triphenylphosphine)-palladium (II) dichloride was stirred for 2 hours and then 500 ml of ice-cooled water were added. The mixture was extracted 3 times with 500 ml of ethyl acetate and the organic phase was washed with salt water, then dried over sodium sulfate, and evaporated under reduced pressure to obtain 136.542 g of a brown oil which was purified by distillation under reduced pressure to obtain 106.979 g of the expected product with a boiling point of 75°-82° C. under 0.2 mbar and a melting point of 62° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05707982 |
| 출처 데이터셋 | uspto-grants-1998_01 |
| ORD ID | ord-020795ec5693400798a1ee4408a40f81 |
| 출처 메모 | uspto-grants-1998_01 |