反应详情

A solution of 5.2 g (24.6 mmol, 46% strength) of 3-cyano-2,5-dihydrofuran in 50 ml of absolute methylene chloride is mixed with 0.3 g of triethylamine and 0.3 g of trifluoroacetic acid, the mixture is heated under reflux and then 7 g (29.5 mmol) of N-benzyl-N-methoxymethyl-N-(trimethylsilylmethyl)-amine are added dropwise. Subsequently, the mixture is heated under reflux for 2 hours and the solution is washed with saturated sodium hydrogen carbonate solution, dried over magnesium sulphate, concentrated and distilled. Yield: 4.5 g (80% of theory). Boiling point: 140°-145° C./0.03 mbar

1. temperaturethe mixture is heated
2. temperatureunder reflux
3. temperatureSubsequently, the mixture is heated
4. temperatureunder reflux for 2 hours
5. washthe solution is washed with saturated sodium hydrogen carbonate solution
6. dry with materialdried over magnesium sulphate
7. concentrationconcentrated
8. distillationdistilled