참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydroquinone | HCID 785 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 2,2,2-Trifluoroethyl trifluoromethanesulfonate | HCID 80366 | — |
| 용매 | Acetone | HCID 180 | — |
| 생성물 | 1,4-Bis(2,2,2-trifluoroethoxy)benzene | HCID 737156 | 88% |
반응 단계
To a mixture of 2.42 moles (334.4 g.) of potassium carbonate, 2.2 moles (510.6 g.) of 2,2,2-trifluoroethyl trifluoromethanesulfonate in 1.02 liters of acetone is added a solution of 1.0 mole (110 g.) of hydroquinone in 1.1 liters of acetone, slowly over a 2 hour period. The reaction is then heated at reflux for 24 hours, the reaction mixture is evaporated, and 2 liters of chloroform and 2 liters of water are added to the residue. The chloroform layer is separated, the aqueous layer is washed twice with 1 liter of chloroform, and the combined chloroform solution is washed with 1 liter of water. The chloroform solution is dried over magnesium sulfate, then concentrated under vacuum. Hexane is added to the residue and the solid product is collected by filtration and washed with hexane. Additional material is collected from the concentrated residues. A yield of 88 percent, 241 g. of 1,4-bis(2,2,2-trifluoroethoxy)benzene, m.p. 75°-77° C. is obtained.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04642384 |
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| 출처 데이터셋 | uspto-grants-1987_02 |
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| ORD ID | ord-0c65e576f7e7433eacfd9b7e42b52547 |
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| 출처 메모 | uspto-grants-1987_02 |
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