HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium methanesulfonate → HCID 22747447, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium methanesulfonate | HCID 638112 | — |
| Reactant | 1,2-Difluoro-3-iodobenzene | HCID 19066658 | — |
| Catalyst | Copper iodide | HCID 83717 | — |
| Solvent | Dimethylacetamide | HCID 31374 | — |
| Product | HCID 22747447 | HCID 22747447 | 72.5% |
Reaction Steps
1,2-Difluoro-3-iodobenzene (1.70 g; 7.08 mmol), 2.17 g (21.2 mmol) of sodium methanesulfonate and 4.03 g (21.2 mmol) of copper iodide were heated with stirring at 111° C. for 20 hours in 50 ml of N,N-dimethylacetamide. The reaction solution was filtered, chloroform was added to the filtrate and the mixture was washed with a saturated aqueous solution of sodium hydrogen carbonate. The organic layer was dried and concentrated and the resulting residue was purified by a silica gel column chromatography (hexane:ethyl acetate=2:1) to give 987 mg (yield: 72%) of 1,2-difluoro-3-methanesulfonylbenzene as a colorless transparent solution.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07687502B2 |
| Source dataset | uspto-grants-2010_03 |
| ORD ID | ord-5ebaa3e9af374c4c97da47c985b54541 |
| Source note | uspto-grants-2010_03 |