HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 58316990, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 2-Iodoxybenzoic acid | HCID 108794 | — |
| Reactant | HCID 58317006 | HCID 58317006 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 58316990 | HCID 58316990 | 100.1% |
Reaction Steps
2,5-Difluoro-N-(2-fluoro-3-hydroxymethyl-phenyl)-benzenesulfonamide (75, 950 mg, 2.99 mmol) and stabilized 2-iodoxybenzoic acid (2.608 g, 45%, 4.2 mmol) are dissolved in 150 mL of tetrahydrofuran and the reaction is stirred at room temperature for 16 hours. The reaction is poured into water and extracted with ethyl acetate. The organic layer is washed with brine, dried over sodium sulfate, filtered and the filtrate is concentrated under vacuum. The resulting material is purified by silica gel column chromatography, eluting with ethyl acetate and dichloromethane. Appropriate fractions are combined and concentrated under vacuum to provide the desired compound (76, 0.944 g). MS (ESI) [M−H+]−=314.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08673928B2 |
| Source dataset | uspto-grants-2014_03 |
| ORD ID | ord-a88499c8ec3245a1b2b770a31b4f6dab |
| Source note | uspto-grants-2014_03 |