HRID34549

反应详情

EQUATION

反应方程式

HRID 34549 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3'-Acetyl-1'-benzyloxymethyl-3-methyl-spiro[1,2,3,4-tetrahydroquinazoline-4,4'-imidazolidine]-2,2',5'trione (3.06 g) is dissolved in dimethylformamide (20 ml) and thereto is added methyl iodide (1 ml) and further added in portions sodium hydride (60%) (0.3 g) under ice-cooling, and the mixture is stirred at room temperature for 30 minutes. To the reaction mixture is added water, and the mixture is extracted with ethyl acetate. The extract is dried and distilled to remove the solvent. The residue is purified by silica gel column chromatography (solvent: chloroform) to give 3'-acetyl-1'-benzyloxymethyl-1,3-dimethyl-spiro[1,2,3,4-tetrahydroquinazoline-4,4'-imidazolidine]-2,2',5'-trione (3 g, yield: 94.5%) as an oily substance.

WORKUP

后处理

  1. temperaturecooling
  2. extractionthe mixture is extracted with ethyl acetate
  3. customThe extract is dried
  4. distillationdistilled
  5. customto remove the solvent
  6. customThe residue is purified by silica gel column chromatography (solvent: chloroform)