Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Water → 2-Fluoro-4-(3-trifluoromethylphenylthio)benzaldehyde
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | 3-(Trifluoromethyl)benzenethiol | HCID 136751 | — |
| 반응물 | 4-Bromo-2-fluorobenzaldehyde | HCID 143517 | — |
| 촉매 | 1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine) | HCID 636044 | — |
| 촉매 | Palladium, tris[mu-[(1,2-eta:4,5-eta)-(1E,4E)-1,5-diphenyl-1,4-pentadien-3-one]]di-, compd. with trichloromethane (1:1) | HCID 11029508 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | 2-Fluoro-4-(3-trifluoromethylphenylthio)benzaldehyde | HCID 58022601 | 68% |
반응 단계
Under an argon atmosphere, ethyldiisopropylamine (7.0 mL), tris(dibenzylideneacetone)dipalladium(0) chloroform adduct (518 mg), xantphos (578 mg), and 3-trifluoromethylthiophenol (3.56 g) were added at room temperature into a solution of 4-bromo-2-fluorobenzaldehyde (4.06 g) in 1,4-dioxane (42 mL), and the resultant solution was heated to reflux for 5 hours. To the reaction solution added water, extracted with ethyl acetate, washed with water and saturated brine in that order, and then dried over anhydrous sodium sulfate. The solvent was evaporated, and the resultant residue was purified by silica gel column chromatography (hexane:ethyl acetate=30:1) to obtain the target product (4.08 g) as a colorless oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08476305B2 |
| 출처 데이터셋 | uspto-grants-2013_07 |
| ORD ID | ord-ba81324ddb7f4c3b85a8c5cb1aea8a62 |
| 출처 메모 | uspto-grants-2013_07 |