Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Sulfate | HCID 24436 | — |
| Reactant | 4-Bromobenzyl alcohol | HCID 70119 | — |
| Reactant | 2,2-Difluoro-2-(fluorosulfonyl)acetic acid | HCID 2737516 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | 1069051-44-0 | HCID 59317853 | 37.1% |
Reaction Steps
To a solution of 4-bromobenzyl alcohol (5.6 g) in acetonitrile (15 ml), sodium sulfate (0.28 g) was added. While warmed to 45° C., 2,2-difluoro-2-(fluorosulfonyl)acetic acid (1.78 g) was slowly dropwise added, and the mixture was heated and refluxed at 45° C. for 4 hours. The reaction solution was poured into water, the mixture was extracted with diethyl ether and the organic layer was washed with water and dried over anhydrous sodium sulfate. The solvent was distilled off in vacuo and the residue obtained was purified with silica gel column chromatography (hexane:ethyl acetate=19:1 to 17:3) to afford the above-identified compound (0.88 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08293781B2 |
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| Source dataset | uspto-grants-2012_10 |
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| ORD ID | ord-5c13996026544dea9693030aad55b6da |
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| Source note | uspto-grants-2012_10 |
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