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
Into an ice cold solution of 4-hydroxy-2-oxo-1-pyrrolidineacetic acid (0.95 g) and 1-(2-aminoacetyl)-2,2-dimethyl-4-imidazolidinone (1 g) in dimethylsulfoxide (30 ml) a solution of DCC (1,22 g) in tetrahydrofuran (10 ml) was added dropwise. The solution was stirred at room temperature overnight and then heated at 50° for 4 hours. After cooling the solution was diluted with water and the resulting precipitate was filtered off. The filtrate was evaporated to dryness under vacuum. The residue was dissolved in water and eluted on a column of Amberlite IR 120H (20 ml). The eluate was treated with Amberlite IRA 68 (10 ml), filtered and evaporated under vacuum. The residue was triturated with isopropanol to yield 0.4 g of the title compound, m.p. 227°-229° .
WORKUP
后处理
- temperatureheated at 50° for 4 hours
- temperatureAfter cooling the solution
- filtrationthe resulting precipitate was filtered off
- customThe filtrate was evaporated to dryness under vacuum
- dissolutionThe residue was dissolved in water
- washeluted on a column of Amberlite IR 120H (20 ml)
- additionThe eluate was treated with Amberlite IRA 68 (10 ml)
- filtrationfiltered
- customevaporated under vacuum
- customThe residue was triturated with isopropanol