HuagongsheHuagongshe Chemistry Print Report · For research reference only
Iodine → HCID 22645647, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Iodine | HCID 807 | — |
| Reactant | HCID 10066685 | HCID 10066685 | — |
| Catalyst | Silver trifluoroacetate | HCID 76299 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 22645647 | HCID 22645647 | — |
Reaction Steps
To a solution of 1-(2,6-dichloro-4-trifluoromethylphenyl)-4-trimethylsilyl-1,2,3-triazole (EP-400842-A1; 1.00 g) in tetrahydrofuran (20 ml) was added silver trifluoroacetate (623 mg) and iodine (716 mg) at -78° C. under an atmosphere of nitrogen. The reaction was allowed to warm to room temperature over 1 hour and then left to stir for a further 16 hours. The reaction was filtered and the filtrate diluted with water (100 ml) and extracted with ether (100 ml), the organic fraction was separarted, dried over MgSO4, filtered and evaporated to dryness. The residue was purified by column chromatography (silica, 100 g) eluted with dichloromethane:hexane (2:1) to give the title compound as a pale yellow crystalline material, m.p. 194-195° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06083965 |
| Source dataset | uspto-grants-2000_07 |
| ORD ID | ord-f7ccfebfe3d74f6798a82425d877d16d |
| Source note | uspto-grants-2000_07 |