참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Benzoyl Peroxide | HCID 7187 | — |
| 반응물 | 2,2-Difluoroethenyl 4-methylbenzene-1-sulfonate | HCID 10977366 | — |
| 반응물 | Sodium Bisulfite | HCID 23665763 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | Sodium 1,1-difluoro-2-tosyloxyethanesulfonate | HCID 86612196 | 16% |
반응 단계
9.3 g of 2,2-difluoroethenyl tosylate, which had been synthesized by a conventional technique, was dispersed in 17 g of water and 37 g of methanol, after which 4.7 g of sodium hydrogen sulfite and 0.5 g of benzoyl peroxide were added. The reaction mixture was stirred at 80° C. for 40 hours. The reaction solution was allowed to cool, after which methanol was distilled off in vacuum. Toluene was added, followed by separatory operation to separate a water layer. A saturated sodium chloride aqueous solution was added to the water layer whereupon white crystals settled out. The crystals were collected by filtration, washed with a small volume of saturated sodium chloride aqueous solution and then dried in vacuum, obtaining the target compound, sodium 1,1-difluoro-2-tosyloxyethanesulfonate. White crystals, 2.5 g (yield 16%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07531290B2 |
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| 출처 데이터셋 | uspto-grants-2009_05 |
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| ORD ID | ord-4691630394ac41cbaeb1d3a0205ceffb |
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| 출처 메모 | uspto-grants-2009_05 |
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