Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Chloroacetone | HCID 6571 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 84662442 | HCID 84662442 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 70979744 | HCID 70979744 | — |
Reaction Steps
1-Chloroacetone (95%, 2.66 g, 27.34 mmol) was added to a stirred solution of 3-fluoro-5-methylsulfonyl-phenol (80%, 1.3 g, 5.46 mmol) and potassium carbonate (2.26 g, 16.40 mmol) in dry dimethyl formamide (10 ml), the mixture was heated to 120° C. for 20 minutes, the mixture was allowed to cool to ambient temperature and water (100 ml) was added. The aqueous phase was extracted with ethyl acetate (3×100 ml), the combined organic phase was washed with LiCl (5% aqueous solution, 4×50 ml), brine (50 ml) and dried with Na2SO4 and evaporated. Purification on flash chromatography (isooctane:ethyl acetate 1:0 to 3:2). 0.905 g, 67%. MS m/z (relative intensity, 70 eV) 246 (M+, 79), 204 (55), 203 (bp), 141 (30), 94 (67).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09120728B2 |
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| Source dataset | uspto-grants-2015_09 |
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| ORD ID | ord-34fb5f3f64cc438d9c6d2d79c79d398b |
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| Source note | uspto-grants-2015_09 |
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