Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Acetic Acid → 2,2-Difluoroethenyl 4-methylbenzene-1-sulfonate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | Ethanol, 2,2,2-trifluoro-, 1-(4-methylbenzenesulfonate) | HCID 67942 | — |
| 반응물 | Butyllithium | HCID 178418339 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 2,2-Difluoroethenyl 4-methylbenzene-1-sulfonate | HCID 10977366 | 47.1% |
반응 단계
Add n-butyllithium (1.6 M in hexanes, 4.9 mL, 7.8 mmol) dropwise over 5 min to a solution of 2,2,2-trifluoroethyl-p-toluene sulfonate (1.0 g, 3.9 mmol) in THF (20 mL) at −78° C. Stir for 30 min, add acetic acid (225 μL, 3.9 mmol) and stir for 30 min. Warm to room temperature, add ethyl acetate and extract with saturated aqueous ammonium chloride, and saturated aqueous sodium bicarbonate. Dry (magnesium sulfate), concentrate and purify (silica gel chromatography, eluting with 0:100 to 15:85 ethyl acetate:hexanes) to give the title compound as an oil (430 mg, 47%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07585885B2 |
| 출처 데이터셋 | uspto-grants-2009_09 |
| ORD ID | ord-1d3857bc200c4ba4b6155d3a47f970d4 |
| 출처 메모 | uspto-grants-2009_09 |