HRID256367

反应详情

EQUATION

反应方程式

HRID 256367 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

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

  1. temperatureheated at 50° for 4 hours
  2. temperatureAfter cooling the solution
  3. filtrationthe resulting precipitate was filtered off
  4. customThe filtrate was evaporated to dryness under vacuum
  5. dissolutionThe residue was dissolved in water
  6. washeluted on a column of Amberlite IR 120H (20 ml)
  7. additionThe eluate was treated with Amberlite IRA 68 (10 ml)
  8. filtrationfiltered
  9. customevaporated under vacuum
  10. customThe residue was triturated with isopropanol