HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lawesson's reagent → HCID 57853827, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lawesson's reagent | HCID 87949 | — |
| Reactant | (2-oxo-2,3,4,5-tetrahydro-1H-benzo[b]azepin-8-yl)-carbamic acid tert-butyl ester | HCID 57853890 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 57853827 | HCID 57853827 | 94.5% |
Reaction Steps
A solution of (2-oxo-2,3,4,5-tetrahydro-1H-benzo[b]azepin-8-yl)-carbamic acid tert-butyl ester (5.0 g, 18.1 mmol) in THF (400 mL) was treated with Lawesson's Reagent (7.5 g, 18.5 mmol). After stirring for 12 hours, the precipitate was removed and the filtrate was concentrated. The residue was purified by silica gel chromatography with DCM to give (2-thioxo-2,3,4,5-tetrahydro-1H-benzo[b]azepin-8-yl)-carbamic acid tert-butyl ester (5.0 g, 17.1 mmol, 94%): MS (m/e) 293 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08552186B2 |
| Source dataset | uspto-grants-2013_10 |
| ORD ID | ord-bea61a9bfa45430ab96e12ecb88750f3 |
| Source note | uspto-grants-2013_10 |