反应详情

温度

-20 °C

4-chlorophenylcarbamate in 100 ml of ether is cooled to −40° C. under an atmosphere of dry nitrogen, 80 ml of a 1.5 M solution of tert-butyllithium in pentane are added dropwise and the mixture is left stirring at −20° C. for 3 hours. The reaction mixture is cooled to −40° C., a solution of 14 g of the compound obtained in step A in 50 ml of THF is added over 1 hour and the mixture is left stirring for 4 days at RT. The reaction mixture is poured into saturated NH4Cl solution and the precipitate formed is spin-filtered off and dried. 10.2 g of the expected product are obtained and are used without further purification in the following step.

1. waitthe mixture is left
2. temperatureThe reaction mixture is cooled to −40° C.
3. waitthe mixture is left
4. stirringstirring for 4 days at RT
5. customthe precipitate formed
6. filtrationis spin-filtered off
7. customdried