참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Catechol | HCID 289 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 2,3-Dichloro-1,1,1,4,4,4-hexafluorobut-2-ene | HCID 9337 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | 2-(1-Chloro-2,2,2-trifluoroethyl)-2-trifluoromethyl-1,3-benzodioxole | HCID 54455048 | — |
반응 단계
110 g of pyrocatechol were dissolved in 1500 ml of acetonitrile, and 200 g of triethylamine were added. 235 g of 2,3-dichloro-1,1,1,4,4,4-hexafluorobut-2-ene were added dropwise to the mixture at 75° C. The reaction mixture was subsequently stirred for 2 hours at 75° C. 1200 ml of the solvent were then distilled off under vacuum and the residue was taken up in 1500 ml of water. The product was extracted with diethyl ether and the organic phase was washed twice with 10% by Weight aqueous sodium hydroxide solution and once with water. After drying over magnesium sulphate, the solution was concentrated and subjected to fractional distillation under vacuum. The yield was 258 g (=84% of theory). The boiling point was 63° C. at 12 mbar. The NMR spectra showed the following characteristic absorptions: 19F NMR: -66.8 and -79.7 ppm. 1H NMR: 4.71 ppm.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05420309 |
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| 출처 데이터셋 | uspto-grants-1995_05 |
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| ORD ID | ord-b405f7ef498546cfae9c3584d4f620c0 |
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| 출처 메모 | uspto-grants-1995_05 |
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