HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lawesson's reagent → HCID 86650271, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lawesson's reagent | HCID 87949 | — |
| Reactant | 5-(2-Fluoro-phenyl)-5-trifluoromethyl-[1,4]oxazepan-3-one | HCID 66665933 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86650271 | HCID 86650271 | 180.6% |
Reaction Steps
To a solution of 5-(2-fluoro-phenyl)-5-trifluoromethyl-[1,4]oxazepan-3-one (1.19 g, 4.29 mmol) in 15 mL THF was added Lawesson's reagent (955 mg, 2.36 mmol). The reaction mixture was stirred at room temperature over night. The mixture was then partitioned between aqueous Na2CO3 solution (2 mol/L) and TBME. The layers were separated, washed with aqueous Na2CO3 solution (2 mol/L), brine and TBME. The combined organic layers were dried over MgSO4.H2O and evaporated. The crude product was purified on a silica gel column by eluting with hexane/EtOAc 95/5->90/10 to give 1.25 g of the title compound as a yellow resin.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08846658B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-238e4b0da008435f96a4f71b787a23d3 |
| Source note | uspto-grants-2014_09 |