HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 68157151, compound → HCID 68158133, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 68157151 | HCID 68157151 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 68158133 | HCID 68158133 | 73% |
Reaction Steps
A solution of {(S)-1-[2-(3-cyanocyclobutylamino)-4-fluorophenylcarbamoyl]-ethyl}carbamic acid tert-butyl ester (0.31 g, 0.83 mmol) in acetic acid (5 mL) was stirred at 70° C. for 16 hours and then at 80° C. for 8 hours. The mixture was concentrated in vacuo and the residue dissolved in DCM then washed with saturated aqueous NaHCO3 and brine, dried (Na2SO4) and concentrated in vacuo. The residue was purified by chromatography (Si—PPC; eluting with ethyl acetate in cyclohexane 0-100%) to give the title compound as colourless gum (0.21 g, 73%). LCMS (Method J): RT 2.87 min [M+H]+ 358.0
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08653089B2 |
| Source dataset | uspto-grants-2014_02 |
| ORD ID | ord-6ddbb8d4335d47559cb13570db07ea07 |
| Source note | uspto-grants-2014_02 |