Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 2,4-Difluorophenol | HCID 123051 | — |
| Reactant | 4-Chloro-2-methyl-1-oxo-1lambda~5~-pyridine | HCID 12211801 | — |
| Solvent | Dimethylacetamide | HCID 31374 | — |
| Product | HCID 14425968 | HCID 14425968 | — |
Reaction Steps
4.3 g (30 mmol) of 4-chloro-2-picoline-N-oxide are added to a mixture of 4.6 g (35 mmol) of 2,4-difluorophenol in 25 ml of N,N-dimethylacetamide and 4.9 g (35 mmol) of finely powdered potassium carbonate and the mixture is warmed to 140° C. for 3 hours with stirring. After cooling, the reaction mixture is poured into 250 ml of water, extracted three times using dichloromethane, and the organic phases are dried over MgSO4 and concentrated. The residue is taken up in dichloromethane and extracted by shaking with saturated aqueous NaCl solution. After drying and freeing from solvent, the extract is brought to crystallization using diisopropyl ether and washed with ethyl acetate. Colorless crystals, m.p. 112°-124° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05114955 |
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| Source dataset | uspto-grants-1992_05 |
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| ORD ID | ord-b2973b95c30a44b5b627e8cff2ec4d62 |
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| Source note | uspto-grants-1992_05 |
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