反应详情

温度

10 °C

Under an inert atmosphere, 7.728 g (118.19 mmoles) of zinc in nanopowder form are suspended in 100 ml of diethyl ether. 5.00 g (29.55 mmoles) of tert-butyl 3-methylene-azetidine-1-carboxylate (WO 2008124085) are added, then the medium is cooled to 10° C. A solution of 6.60 ml (59.09 mmoles) of trichloroacetyl chloride in ml of 1,2-dimethoxyethane is added drop by drop while maintaining the temperature of the reaction medium between 26 and 30° C. After stirring for 14 hrs at ambient temperature, the medium is filtered over celite, the celite is copiously rinsed with diethyl ether and the filtrate is partially concentrated under reduced pressure. The crude reaction product thus obtained is used as such in the following stage.

1. temperaturewhile maintaining the temperature of the reaction medium between 26 and 30° C
2. filtrationthe medium is filtered over celite
3. washthe celite is copiously rinsed with diethyl ether
4. concentrationthe filtrate is partially concentrated under reduced pressure
5. customThe crude reaction product
6. customthus obtained