Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 2-Methyl-3-nitrophenol | HCID 79579 | — |
| Reactant | Sodium chlorodifluoroacetate | HCID 2734985 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 1383974-37-5 | HCID 86699283 | — |
Reaction Steps
A solution of 10 g of 2-methyl-3-nitrophenol in 20 ml of N,N-dimethylformamide is added to a mixture of 23.4 g of sodium chlorodifluoroacetate and 22 g of potassium carbonate in 30 ml of N,N-dimethylformamide and 6 ml of water. The reaction mixture is then heated at 110° C. for 3 hours and left to stand for 16 hours, and then treated with a mixture of water and ethyl acetate. The organic phase is washed with 1N sodium hydroxide, water and a saturated sodium chloride solution, dried over magnesium sulfate, filtered, and concentrated under reduced pressure, so as to give the expected product in the form of a brown oil, used as it is in the next step.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09133168B2 |
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| Source dataset | uspto-grants-2015_09 |
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| ORD ID | ord-db833892bcb44212b36e7746d38f582b |
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| Source note | uspto-grants-2015_09 |
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