HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 68157210, compound → HCID 58459222, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 68157210 | HCID 68157210 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 58459222 | HCID 58459222 | 86.5% |
Reaction Steps
A solution of [(S)-1-(5-fluoro-2-phenylaminophenylcarbamoyl)ethyl]carbamic acid tert-butyl ester (2.15 mmol) in AcOH (10 mL) was stirred for 18 h at 70° C. After cooling to RT, the volatiles were evaporated in vacuo and the residue partitioned between EtOAc and a saturated aqueous solution of NaHCO3. The organic fraction was washed with brine, dried (MgSO4) and concentrated in vacuo. The resulting residue was purified by column chromatography (Si—PCC, gradient 0-40% EtOAc in cyclohexane) to afford the title compound as an orange oil (661 mg, 86% over two steps). LCMS (Method J): RT 3.52 min [M+H]+ 356.1.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08653089B2 |
| Source dataset | uspto-grants-2014_02 |
| ORD ID | ord-fbf7809cc1354e39b4144b5fc483c8db |
| Source note | uspto-grants-2014_02 |