反应详情

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).

1. temperaturethe reaction mixture then heated at 65° C. for 2 h
2. temperatureAfter cooling back to room temperature the solvents
3. customwere removed under reduced pressure
4. customFollowing azeotroping with benzene
5. dissolutionthe residue was dissolved in ether
6. additiontreated with an excess of cold 1M HCl in ether
7. filtrationThe hydrochloride salt of the title compound was filtered off
8. washwashed well with ether and dichloromethane
9. customDrying
10. customgave a white powder