Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrogen Peroxide | HCID 784 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | HCID 11583112 | HCID 11583112 | — |
| Solvent | Trifluoroacetic acid | HCID 6422 | — |
| Product | HCID 11619554 | HCID 11619554 | 33.7% |
Reaction Steps
Hydrogen peroxide (278 mg, 35%, 2.9 mmol) was added to solution of 5-amino-1-(2,6-dichloro-4-trifluoromethylphenyl)-2,3-dicyano-4-trifluoromethylthiopyrrole (850 mg, 1.9 mmol) in trifluoroacetic acid (10 ml). The resulting solution was stirred at 20° C. for 0.75 hour. Another portion of hydrogen peroxide ( 0.97 mmol) was added and the mixture stirred at 20° C. for a further hour. The reaction mixture was poured into methylene chloride (60 ml) and water (60 ml) and the organic layer washed with water (2×), dried (sodium sulfate), concentrated and purified by chromatography on silica gel, eluting with heptane/ethyl acetate (4:1) to give the title compound as a yellow solid (293 mg, 0.64 mmol); 19F-NMR: −64.35, −75.59.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07674474B2 |
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| Source dataset | uspto-grants-2010_03 |
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| ORD ID | ord-5ead847c14274dbb8394e6285608cab3 |
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| Source note | uspto-grants-2010_03 |
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