反应详情

To a solution of 0.405 g (1 mmol) of methyl (3,5-difluorophenyl)[1-(diphenylmethyl)azetidin-3-ylidene]acetate in 2 mL of dry THF was added 0.284 g (2 mmol) of 1-chloroethyl chloroformate and the solution was stirred at room temperature. After 1 h, the solution was concentrated and the residue was triturated with 2 mL of 10% ether-hexane. This was decanted and the solid residue was dissolved in methanol and heated to reflux for 6 h. The solution was concentrated to afford the title compound as the hydrochloride salt: Mass Spectrum: m/e=240 (M+1).

1. concentrationthe solution was concentrated
2. customthe residue was triturated with 2 mL of 10% ether-hexane
3. customThis was decanted
4. dissolutionthe solid residue was dissolved in methanol
5. temperatureheated
6. temperatureto reflux for 6 h
7. concentrationThe solution was concentrated