HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → HCID 46208244, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | HCID 66995363 | HCID 66995363 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 46208244 | HCID 46208244 | 64% |
Reaction Steps
To a stirred solution of tert-butyl 3-(2,3-difluorophenyl)-3-methoxyazetidine-1-carboxylate (0.7 g, 2.34 mmol) in dichloromethane (20 mL) was added trifluoroacetic acid (3 ml, 40 mmol). The resulting mixture was stirred at ambient temperature for 2 h. The solvent was evaporated and the crude product was purified on a Biotage Isolute SCX-3 SPE column (washed with methanol and eluted with methanol/triethylamine, 4:1). The solvents where evaporated to give (0.16 g, 64%) of the title compound. The amine was converted to the oxalic acid salt and recrystallized from ethanol/diethyl ether/diisopropyl ether: M.p. 141-142° C. MS m/z (relative intensity, 70 eV) 199 (M+, 1), 170 (bp), 169 (97), 140 (82), 127 (47).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08586572B2 |
| Source dataset | uspto-grants-2013_11 |
| ORD ID | ord-307d3c8db290418f8e01279314285f56 |
| Source note | uspto-grants-2013_11 |