HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 68157224, compound → HCID 68157429, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 68157224 | HCID 68157224 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 68157429 | HCID 68157429 | 86% |
Reaction Steps
A solution of {(S)-1-[2-(3-cyanophenylamino)phenylcarbamoyl]ethyl}carbamic acid tert-butyl ester (289 mg, 0.75 mmol) in AcOH (3 mL) was heated at 80° C. for 16 h. After cooling to RT, the volatiles were removed in vacuo and the residue dissolved in DCM and washed with a saturated aqueous solution of NaHCO3. The aqueous phase was further extracted with DCM (×3) and the combined organic fractions were dried (Na2SO4) and concentrated in vacuo. The resulting residue was purified by column chromatography (Si—PCC, gradient 0-2% 2M NH3/MeOH in DCM) to afford the title compound (232 mg, 86%). The material was still impure and taken forward in the next step without further purification. LCMS (Method C): RT 3.54 min [M+H]+ 363.4
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08653089B2 |
| Source dataset | uspto-grants-2014_02 |
| ORD ID | ord-d51cfdd7d54046289365f504f06c1485 |
| Source note | uspto-grants-2014_02 |