HRID53875
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 40 °C
PROCEDURE
实验过程
14.4 g (0.15 mol) of 4,5-dihydrofuran-2-carbonitrile are introduced in 300 ml of absolute methylene chloride, 1.8 g of triethylamine and 1.8 g of trifluoroacetic acid are added, and the mixture is warmed to 40° C. 42.6 g (0.15 mol) of N-benzyl-N-methoxymethyl-N-trimethylsilylmethylamine are added dropwise to this mixture which is then stirred at 40° C. for 15 hours. It is then washed with 50 ml of saturated sodium hydrogen carbonate solution, dried over MgSO4, concentrated and distilled twice. Yield: 9.3 g (22.5% of theory) Boiling point: 120°-125° C./0.06 mbar The product is 83% pure by gas chromatography.
WORKUP
后处理
- washIt is then washed with 50 ml of saturated sodium hydrogen carbonate solution
- dry with materialdried over MgSO4
- concentrationconcentrated
- distillationdistilled twice