HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → HCID 58318661, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | HCID 58318672 | HCID 58318672 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 58318661 | HCID 58318661 | 100% |
Reaction Steps
TFA (2 ml) was added over a period of 5 minutes to a stirred solution of tert-butyl (2R,4R)-2-(aminocarbonyl)-4-({4-[(3-chloro-2-fluorophenyl)amino]-7-methoxyquinazolin-6-yl}oxy)piperidine-1-carboxylate (0.13 g, 0.232 mmol) in DCM (2 ml) at 0° C., was added. The reaction mixture was allowed to warm to room temperature and stirred for 1 hour after which time, the reaction was complete. The reaction mixture was concentrated to dryness, azeotroped twice with toluene and the residue was purified by flash chromatography (silica gel, DCM-NH3/MeOH 5%) to give (2R,4R)-4-({4-[(3-chloro-2-fluorophenyl)amino]-7-methoxyquinazolin-6-yl}oxy)piperidine-2-carboxamide (9) (0.102 g, 100%) as a yellow solid; Mass Spectrum: (M+H)+ 446.1.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08735410B2 |
| Source dataset | uspto-grants-2014_05 |
| ORD ID | ord-ac6529183db34f8d94bd5ace3a4ec778 |
| Source note | uspto-grants-2014_05 |