Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Epichlorohydrin | HCID 7835 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 2,4-Difluoro-6-nitrophenol | HCID 223083 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 18520594 | HCID 18520594 | — |
Reaction Steps
A mixture consisting of 12.62 g of 2,4-difluoro-6-nitrophenol, 36 ml of epichlorohydrin, 3.3 g of sodium hydroxide, 15 ml of water and 320 ml of ethanol was stirred at 80° C. for 24 hours. After cooling the reaction solution to room temperature, the insoluble matter was removed by filtration and the filtrate was concentrated to dryness under a reduced pressure. The resulting residue was dissolved in an ether-hexane (1:2) mixed solvent, washed with water and saturated brine and dried with anhydrous sodium sulfate, and then the solvent was evaporated under a reduced pressure. The residue was applied to a silica gel column chromatography and developed with an ethyl acetate-hexane (1:9) mixed solvent, and then the fractions containing the compound of interest were concentrated to obtain 11.28 g of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06573377B1 |
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| Source dataset | uspto-grants-2003_06 |
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| ORD ID | ord-466d72e675f14be484a4116b56d017e2 |
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| Source note | uspto-grants-2003_06 |
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