Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrochloric Acid → 3,4,4-Trifluoro-3-butenoic acid, 4-nitrophenyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 4-Nitrophenol | HCID 980 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 3,4,4-Trifluoro-3-butenoyl chloride | HCID 10920789 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 생성물 | 3,4,4-Trifluoro-3-butenoic acid, 4-nitrophenyl ester | HCID 15239190 | 92.1% |
반응 단계
A solution of 4-nitrophenol (1.10 g, 0.0079 mole) and 3,4,4-trifluoro-3-butenoyl chloride (1.85 g, 0.0116 mole) in dry ether (15 mL) is treated dropwise with triethylamine (1.01 g, 0.01 mole) at -78° C. with stirring. The mixture is stirred at -78° C. for 10 min and allowed to reach room temperature. The reaction mixture is diluted with ether (20 mL), stirred with 15 mL of 2 N HCl. The organic layer is successively washed with water, 5% sodium bicarbonate, brine, and dried. The dark brown residue obtained after evaporation of the solvent was purified by passing through a short column of silica gel to give 1.9 g of the product as a brown solid, a 91% yield. m.p. 58°-62° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05623084 |
| 출처 데이터셋 | uspto-grants-1997_04 |
| ORD ID | ord-760aa76627d84edfb1a7dfe8d27792cc |
| 출처 메모 | uspto-grants-1997_04 |