HuagongsheHuagongshe Chemistry Print Report · For research reference only
3,5-Dichlorobenzenesulfonyl chloride → HCID 18626128, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3,5-Dichlorobenzenesulfonyl chloride | HCID 522388 | — |
| Reactant | HCID 10755041 | HCID 10755041 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 18626128 | HCID 18626128 | 94.4% |
Reaction Steps
A solution of 3-amino-4-methoxy-N-(3,4-difluorophenyl)-benzamide from Example 15 (0.834 g, 3.00 mmol), 3,5-dichlorobenzenesulfonyl chloride (0.736 g, 3.00 mmol) and a catalytic amount of 4-dimethylaaminopyridine in pyridine (10 mL) was stirred under nitrogen at room temperature. After 16 hours, the solvent was removed in vacuo and the residue shaken with a mixture of ethyl acetate and 1N HCl then filtered. The layers were separated and the organic layer washed with brine, dried with MgSO4, concentrated to dryness, triturated in hexanes and filtered to afford a solid which was combined with that obtained in the filtration step to afford the product (1.38 g); m.p. 228-231° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06528528B2 |
| Source dataset | uspto-grants-2003_03 |
| ORD ID | ord-69937c81888947708fdc3ba93482a5a0 |
| Source note | uspto-grants-2003_03 |