HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 2-(2,2,2-Trifluoroethoxy)-5-chlorobenzylamine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | HCID 22464525 | HCID 22464525 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 2-(2,2,2-Trifluoroethoxy)-5-chlorobenzylamine | HCID 22464507 | — |
Reaction Steps
To a solution of 2-(2,2,2-trifluoroethoxy)-5-chlorobenzyl azide (1.76 g, 6.63 mmol) in THF (20 mL) was added triphenylphosphine (2 g, 7.63 mmol). After stirring at room temperature for 2 h, water (0.5 mL) was added and the reaction mixture then heated at 65° C. for 2 h. After cooling back to room temperature the solvents were removed under reduced pressure. Following azeotroping with benzene, the residue was dissolved in ether and treated with an excess of cold 1M HCl in ether. The hydrochloride salt of the title compound was filtered off and washed well with ether and dichloromethane. Drying gave a white powder: 1H NMR (CD3OD) δ7.46 (m, 2H), 7.18 (d, J=8.4 Hz, 1H), 4.70 (q, J=8.4 Hz, 2H), 4.14 (s, 2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06387911B1 |
| Source dataset | uspto-grants-2002_05 |
| ORD ID | ord-7ac93e1859a4457295acba98dc753a1e |
| Source note | uspto-grants-2002_05 |