HRID434544

反应详情

EQUATION

反应方程式

HRID 434544 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

19.4 g of 7-hydroxy-5-carboxymethyl-1,2,4-triazolo[1,5-a]pyrimidine and 12 g of hydroxyethylacrylate were dissolved in 150 ml of dimethylformamide (DMF) and thereto, a solution of 20.6 g of N,N-dicyclohexylcarbodiimide in 30 ml of DMF was added dropwise at a room temperature for 10 minutes. Thereafter, stirring was continued at a room temperature for 8 hours, and the precipitate produced was removed by filtration. The filtrate was condensed under a reduced pressure and low temperature. The thus obtained residue was chromatographed through silica gel put in a column in order to separate it into components and purify. The intended compound was obtained in a form of crystal. It was recrystallized from ethyl acetate. Thus, 6 g of white crystal having a melting point of 108° to 109° C. (intended compound) was obtained.

WORKUP

后处理

  1. customthe precipitate produced
  2. customwas removed by filtration
  3. customcondensed under a reduced pressure and low temperature
  4. customThe thus obtained residue was chromatographed through silica gel
  5. customto separate it into components
  6. custompurify
  7. customThe intended compound was obtained in a form of crystal
  8. customIt was recrystallized from ethyl acetate
  9. customwas obtained