Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Water → Methyl 2-((trimethylsilyl)ethynyl)benzoate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Trimethylsilylacetylene | HCID 66111 | — |
| 반응물 | Methyl 4-iodobenzoate | HCID 69273 | — |
| 촉매 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | Methyl 2-((trimethylsilyl)ethynyl)benzoate | HCID 11053512 | 100.2% |
반응 단계
20.60 g (78.61 mmol) of 4-Iodobenzoic acid methyl ester and 9.26 g (94.33 mmol) of ethynyl trimethylsilane were dissolved in 200 ml of tetrahydrofuran, and thereto 23.86 g (235.83 mmol) of triethylamine, 1.65 g (2.36 mmol) of dichloro(bistriphenylphosphine)palladium(II) and 0.45 g (2.36 mmol) of copper(I) iodide were added. The mixture was stirred at room temperature for 8 hours. At the end of reaction, added water and extracted with ethylacetate. The extract was washed with saturated sodium chloride solution, dried over anhydrous magnesium sulfate, and separated by column chromatography to obtain trimethylsilylethynylbenzoic acid methyl ester 18.30 g (Yield 100%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08349885B2 |
| 출처 데이터셋 | uspto-grants-2013_01 |
| ORD ID | ord-a38fee4a0dc94c7694a1e30f0d4038ba |
| 출처 메모 | uspto-grants-2013_01 |