HuagongsheHuagongshe Chemistry Print Report · For research reference only
Boron tribromide → HCID 57750987, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Boron tribromide | HCID 25134 | — |
| Reactant | HCID 68779175 | HCID 68779175 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 57750987 | HCID 57750987 | 99.1% |
Reaction Steps
To a solution of 2-(2,3-dichloro-benzenesulfonylamino)-5-methoxy-benzenesulfonamide (4.8 g, 11.68 mmol) in DCM (200 mL) at −20° C., BBr3 (1M in DCM, 60 mL, 60 mmol) was added dropwise over 30 minutes. The reaction mixture was allowed to warm to RT and the stirring was continued overnight. The reaction mixture was then cooled to −20° C., quenched by addition of methanol (20 mL) and volatiles were removed under reduced pressure. The residue was partitioned between water (50 mL) and ethyl acetate (100 mL). The organic phase was washed with water, dried over sodium sulfate and concentrated under reduced pressure. The crude product was recrystallized from methanol to afford the title compound (4.6 g, 65%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09145380B2 |
| Source dataset | uspto-grants-2015_09 |
| ORD ID | ord-ccf7fd76ba8f4193bac5cbe9efd2e8c3 |
| Source note | uspto-grants-2015_09 |