Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 1-Ethylpiperazine | HCID 79196 | — |
| Reactant | 4-Chloro-2,3-difluoro-6-nitroaniline | HCID 17897329 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | HCID 21911983 | HCID 21911983 | 63.1% |
Reaction Steps
To a solution of 768 mg of 4-chloro-2,3-difluoro-6-nitroaniline (which was prepared by the method described in WO 98/56761 or WO 98/35977) and 629 mg of 1-ethylpiperazine in 5 ml of dimethylsulfoxide, 1.00 g of potassium carbonate was added, followed by 2 hours' stirring at 50° C. Water was added to the reaction liquid, followed by extraction with ethyl acetate. The ethyl acetate layer was washed with saturated brine, dried on anhydrous magnesium sulfate, and the solvent was distilled off. The residue was separated and purified on silica gel column chromatography (chloroform/methanol=50/1) to provide 704 mg of the title compounds.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07125877B2 |
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| Source dataset | uspto-grants-2006_10 |
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| ORD ID | ord-a44dc534961245dab70e818790206b4c |
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| Source note | uspto-grants-2006_10 |
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