Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Iodine | HCID 807 | — |
| Reactant | HCID 15420923 | HCID 15420923 | — |
| Solvent | Sulfuric Acid | HCID 1118 | — |
| Product | HCID 60136710 | HCID 60136710 | 86.2% |
Reaction Steps
Iodine (30 g) was dissolved in 60% sulfuric acid (fuming, 80 g), and 1,3-dimethyl-5-trifluoromethylpyrazole (13.12 g, 80 mmol) was slowly added under ice-cooling. The mixture was stirred at 0° C. for 2 hr. The reaction mixture was poured into ice water and extracted with ethyl acetate. The organic layer was washed with aqueous sodium thiosulfate and saturated brine, dried over magnesium sulfate and concentrated under reduced pressure. The obtained crude crystals were washed with hexane to give the desired compound (20 g) as crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08404861B2 |
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| Source dataset | uspto-grants-2013_03 |
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| ORD ID | ord-d3c7fcf90721488fbc0c2d724984319d |
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| Source note | uspto-grants-2013_03 |
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