HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → HCID 67264883, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | HCID 67264998 | HCID 67264998 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Solvent | Ammonium Acetate | HCID 517165 | — |
| Product | HCID 67264883 | HCID 67264883 | 75% |
Reaction Steps
Heat a solution of 4-{((R)-1-benzyloxycarbonyl-piperidin-3-yl)-[2-(4-fluoro-3-trifluoromethyl-phenyl)-2-oxo-ethyl]-carbamoyl}-piperidine-1-carboxylic acid tert-butyl ester (4.40 mmol; 2.86 g) in DMF (2.5 mL) and ammonium acetate saturated in acetic acid (15 mL) at 90° C. for 8 h. Dilute with EA, wash the organic phase 3× with water, saturated sodium bicarbonate, brine, dry over MgSO4 and filter. Purify the residue on 80 g silica gel with 5-20% EA/DCM to provide the title compound (2.08 g; 3.30 mmol; 75%). MS (ES+): m/z=631 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08148387B2 |
| Source dataset | uspto-grants-2012_04 |
| ORD ID | ord-1e6d261bea3e436ebb18c7d4f6ee9ea0 |
| Source note | uspto-grants-2012_04 |