HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylamine → 4-bromo-2-fluoro-N,N-dimethylbenzenesulfonamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylamine | HCID 674 | — |
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 4-Bromo-2-fluorobenzene-1-sulfonyl chloride | HCID 2736310 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 4-bromo-2-fluoro-N,N-dimethylbenzenesulfonamide | HCID 59206747 | 75% |
Reaction Steps
To 4-bromo-2-fluorobenzene-1-sulfonyl chloride (1.0 g, 3.7 mmol) and Et3N (1.5 mL, 11 mmol) in dichloromethane (10 mL) was added a solution of dimethylamine 2.0 M in THF (2.2 mL, 4.4 mmol). The reaction was stirred at ambient temperature for 30 minutes. The reaction was washed with 10 mL of 1N aqueous HCl and 10 mL of brine. Organics were dried over Na2SO4 and evaporated to dryness. Crude product was purified by chromatography on silica gel (eluting with 0-25% ethyl acetate in hexanes) to afford 4-bromo-2-fluoro-N,N-dimethylbenzenesulfonamide (780 mg, 75%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08846753B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-3e0b2a28cb8c4daf9445f3578e7c0b79 |
| Source note | uspto-grants-2014_09 |