Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → 2-(p-Chlorophenyl)-4-phenyl-5-(trifluoromethyl)-3-[(trifluoromethyl)sulfonyl]pyrrole
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 5(2H)-Oxazolone, 4-(4-chlorophenyl)-2-(trifluoromethyl)- | HCID 11065291 | — |
| 반응물 | [2,2-Bis(trifluoromethanesulfonyl)ethenyl]benzene | HCID 18930436 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Water ethylacetate | HCID 22728543 | — |
| 생성물 | 2-(p-Chlorophenyl)-4-phenyl-5-(trifluoromethyl)-3-[(trifluoromethyl)sulfonyl]pyrrole | HCID 18930408 | — |
반응 단계
A solution of 4-(p-chlorophenyl)-2-(trifluoromethyl)-3-oxazolin-5-one (1.0 g, 3.8 mmol) and β,β-bis[(trifluoromethyl)sulfonyl]styrene (1.4 g, 3.8 mmol) in dimethylformamide is stirred for two hours at 110° C., treated with triethylamine (0.38 g, 3.8 mmol), stirred for several hours at reflux and diluted with an ethyl acetate/water mixture. The organic phase is separated, washed with water and dilute hydrochloric acid, dried over anhydrous magnesium sulfate and concentrated in vacuo to obtain a residue. Chromatography of the residue using silica gel and a 1:10 ethyl acetate/hexanes solution gives the title product as an amber oil which is identified by 1HNMR and 13CNMR spectral analyses.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05468877 |
| 출처 데이터셋 | uspto-grants-1995_11 |
| ORD ID | ord-822e80ae85f146fb9e22c89eea073838 |
| 출처 메모 | uspto-grants-1995_11 |