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
9.6 g of tert.-butyl (4S)-3-benzyloxycarbonyl-2-oxo-imidazolidine-4-carboxylate are dissolved in 200 ml of dimethylformamide, and 14.0 g of silver oxide are added thereto. 42.6 g of methyl iodide are added to the mixture at room temperature under stirring, and the mixture is further stirred for 2 days in the dark. The reaction mixture is filtered to remove insoluble materials, and the filtrate is concentrated under reduced pressure. The residue obtained is dissolved in ethyl acetate. Then, the ethyl acetate solution is washed with water, dried and concentrated under reduced pressure. The residue thus obtained is washed with n-hexane. 8.45 g of tert.-butyl (4S)-1-methyl-3-benzyloxycarbonyl-2-oxo-imidazolidine-4-carboxylate are thereby obtained as colorless crystals. Yield: 84.3%
WORKUP
后处理
- stirringthe mixture is further stirred for 2 days in the dark
- filtrationThe reaction mixture is filtered
- customto remove insoluble materials
- concentrationthe filtrate is concentrated under reduced pressure
- customThe residue obtained
- washThen, the ethyl acetate solution is washed with water
- customdried
- concentrationconcentrated under reduced pressure
- customThe residue thus obtained
- washis washed with n-hexane