HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Anhydride → N-acetyl-5-bromo-3-formyl-4-methoxybenzenesulfonamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 3-Bromo-5-formyl-4-methoxy-benzenesulfonamide | HCID 86607698 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | N-acetyl-5-bromo-3-formyl-4-methoxybenzenesulfonamide | HCID 86607697 | 91.6% |
Reaction Steps
A 100 mL round-bottom flask was charged with 5-bromo-3-formyl-4-methoxy-benzenesulfonamide (586 mg, 2.0 mmol) dissolved in dichloromethane (40 mL) and the solution was stirred vigorously while triethylamine (252 mg, 2.50 mmol) was added, followed by acetic anhydride (224 mg, 2.2 mmol) and a catalytic amount of N,N-dimethylaminopyridine. The mixture was stirred for 1 hour and then concentrated by evaporation. The residue was partitioned between 5% citric acid and ethyl acetate. The organic layer was separated, washed with water and brine and dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure to give N-acetyl-5-bromo-3-formyl-4-methoxybenzenesulfonamide (616 mg) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08778625B2 |
| Source dataset | uspto-grants-2014_07 |
| ORD ID | ord-3b282f7e76cc436aab302183e3c232fa |
| Source note | uspto-grants-2014_07 |