HRID458679

反应详情

EQUATION

反应方程式

HRID 458679 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of intermediate 4, 6-benzyloxy-2,5-dioxo-1,2,3,5-tetrahydro-imidazo[1,2-a]pyrimidine-7-carboxylic acid ethyl ester, (0.770 g, 2.34 mmol) in trifluoroacetic acid (20 ml) was stirred at 25° C. for 1 h. The solvent was then evaporated under reduced pressure and residual trifluoroacetic acid removed by azeotropic distillation with toluene in vacuo. Acetic acid (5 ml) was added and the mixture subjected to azeotropic distillation with toluene in vacuo to remove solvent and residual acid. Recrystallization of the solid residue from ethyl acetate gave 0.497 g (88% yield) of the title ester as white crystals; mp 265° C. (dec).

WORKUP

后处理

  1. customThe solvent was then evaporated under reduced pressure and residual trifluoroacetic acid
  2. customremoved by azeotropic distillation with toluene in vacuo
  3. additionAcetic acid (5 ml) was added
  4. distillationthe mixture subjected to azeotropic distillation with toluene in vacuo
  5. customto remove solvent and residual acid
  6. customRecrystallization of the solid residue from ethyl acetate