HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 4-((4-Fluorotetrahydro-2h-pyran-4-yl)methoxy)-3-(trifluoromethylsulfonyl)benzenesulfonamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 4-Fluoro-3-((trifluoromethyl)sulfonyl)benzenesulfonamide | HCID 25058452 | — |
| Reactant | (4-Fluorooxan-4-yl)methanol | HCID 56971676 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 4-((4-Fluorotetrahydro-2h-pyran-4-yl)methoxy)-3-(trifluoromethylsulfonyl)benzenesulfonamide | HCID 67126545 | — |
Reaction Steps
To a solution of EXAMPLE 37C (0.500 g) in tetrahydrofuran (5 mL) was added sodium hydride (0.596 g). Additional tetrahydrofuran (25 mL) was added and the mixture stirred for 30 minutes, then 4-fluoro-3-(trifluoromethylsulfonyl)benzenesulfonamide (1.145 g) was added as a solution in tetrahydrofuran (5 mL). After stirring for 2 hours, the reaction mixture was partioned between 1N aqueous HCl (50 mL) and dichloromethane (200 mL). The organic layer was dried over magnesium sulfate, filtered, and concentrated. The resulting solid was chromatographed over silica gel (Reveleris 80 g) eluting with a gradient of 0.5% to 7.5% methanol/dichloromethane over 30 minutes (flow=40 mL/min) to provide the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09045475B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-a7c0809171864779a6d81c7c88685671 |
| Source note | uspto-grants-2015_06 |