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
A cold (0° C.) solution of 3-benzyl-2,2-dimethylimidazolidin-4 -one (2.28 g, 11.16 mmol) in CH2Cl2 (25 mL) was treated with benzylchloroformate (0.96 mL, 6.70 mmol), a solution of 4-dimethylaminopyridine (1.71 g, 13.95 mmol) in CH2Cl2 (10 mL), and again with benzylchloroformate (0.96 mL, 6.70 mmol). The solution was stirred for 30 min and poured into aqueous 10% KHSO4 solution. The layers were separated, and the organic was washed twice with water and once with brine. The organic layer was dried over Na2SO4, filtered, and concentrated in vacuo to afford an orange oil. The oil was treated with Et2O causing a precipitate which was filtered to afford the product as a white solid. 1H NMR (400 MHz, CDCl3) δ 7.37 (m, 10H), 5.14 (s, 2H), 4.54 (s, 2H), 4.11 (s, 6H), 1.56 (s, 6H); ES MS (M+1)=339.
WORKUP
后处理
- customThe layers were separated
- washthe organic was washed twice with water and once with brine
- dry with materialThe organic layer was dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated in vacuo
- customto afford an orange oil
- filtrationwas filtered