HuagongsheHuagongshe Chemistry Print Report · For research reference only
Iodine → HCID 58542540, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Iodine | HCID 807 | — |
| Reactant | Ammonium cerium (IV) nitrate | HCID 9869224 | — |
| Reactant | HCID 58542532 | HCID 58542532 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 58542540 | HCID 58542540 | — |
Reaction Steps
A solution of 500 mg (2.42 mmol) of methyl 3-(difluoromethoxy)-1-methyl-1H-pyrazole-5-carboxylate in 20 ml of acetonitrile is admixed with 665 mg (1.21 mmol) of ammonium cerium(IV) nitrate and 369 mg (1.45 mmol) of iodine and heated under reflux for three hours and afterstirred at room temperature overnight. The reaction mixture is diluted with water and ethyl acetate, and the organic phase is washed with saturated sodium thiosulphate solution, dried over sodium sulphate, filtered and concentrated by evaporation in vacuo. This gives 750 mg of methyl 3-(difluoromethoxy)-4-iodo-1-methyl-1H-pyrazole-5-carboxylate (93%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08946234B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-95cbc3afe4c842f3a7e971626efbd833 |
| Source note | uspto-grants-2015_02 |