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
PROCEDURE
实验过程
The mixture of 4-(1,1-diphenyl-methoxymethyl)-piperidine (0.760 g, 2.7 mmol, 1.0 eq.), N-(2-bromoethyl)phthalimide (0.686 g, 2.7 mmol, 1.0 eq.), K2CO3 (0.560 g, 4.1 mmol, 1.5 eq.), and NaI (0.567 g, 3.8 mmol, 1.4 eq.) in 2-butanone (10 ml) was refluxed for 2-3 hours. The mixture was then cooled to room temperature. The white solid was filtered off and was washed with small amount of CHCl3. The filtrates were combined and concentrated. The resulted residue was dissolved in CHCl3 (80 ml). The solution was washed with water (3×10 ml), then dried over anhydrous Na2SO4. After removed all solvent, the crude product 2-{2-[4-(1,1-diphenyl-methoxymethyl)-piperidin-1-yl]-ethyl}-isoindole-1,3-dione was yielded (0.980 g, 79.8% yield).
WORKUP
后处理
- temperaturewas refluxed for 2-3 hours
- filtrationThe white solid was filtered off
- washwas washed with small amount of CHCl3
- concentrationconcentrated
- dissolutionThe resulted residue was dissolved in CHCl3 (80 ml)
- washThe solution was washed with water (3×10 ml)
- dry with materialdried over anhydrous Na2SO4
- customAfter removed all solvent