HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chlorosulfonic acid → 2,4-Difluoro-3-methylbenzenesulfonyl chloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chlorosulfonic acid | HCID 24638 | — |
| Reactant | 1,3-Difluoro-2-methylbenzene | HCID 581493 | — |
| Solvent | Water | HCID 962 | — |
| Product | 2,4-Difluoro-3-methylbenzenesulfonyl chloride | HCID 15725375 | 98% |
Reaction Steps
To 1,3-difluoro-2-methylbenzene (5.00 g, 39.0 mmol), chlorosulfuric acid (10.5 mL, 158 mmol) was added with cooling on ice, and the mixture was stirred at room temperature for 5 hours. To the reaction solution, water (100 mL) was added with cooling on ice, followed by extraction with dichloromethane (100 mL). The thus obtained organic layer was dried over anhydrous sodium sulfate. After vacuum concentration, the residue was purified with silica gel chromatography to yield the title compound (8.65 g, 98%) as a colorless amorphous solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08889741B2 |
| Source dataset | uspto-grants-2014_11 |
| ORD ID | ord-897fe641414d4a7faf9fbd47220992ae |
| Source note | uspto-grants-2014_11 |