HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lawesson's reagent → 5-(5-Bromo-2-fluorophenyl)-6,6-difluoro-5-methyl-1,4-oxazepane-3-thione
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lawesson's reagent | HCID 87949 | — |
| Reactant | 5-(5-Bromo-2-fluorophenyl)-6,6-difluoro-5-methyl-1,4-oxazepan-3-one | HCID 66666057 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 5-(5-Bromo-2-fluorophenyl)-6,6-difluoro-5-methyl-1,4-oxazepane-3-thione | HCID 86650273 | — |
Reaction Steps
To a solution of 5-(5-bromo-2-fluorophenyl)-6,6-difluoro-5-methyl-1,4-oxazepan-3-one (2.0 g, 5.93 mmol) in THF (25 mL) was added Lawesson's reagent (2.87 g, 7.1 mmol) at rt and heated to reflux temperature for 16 h. Reaction mixture was concentrated under reduced pressure and directly purified by column chromatography on silica gel using 4% ethyl acetate in Hexane to furnish title compound as colorless gum. Yield=1.0 g (50%). LCMS: RtH8=1.75 [M+H]+=354.8, 355.7,
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08338413B1 |
| Source dataset | uspto-grants-2012_12 |
| ORD ID | ord-9c60e42e3902461ca607f32532778d0e |
| Source note | uspto-grants-2012_12 |