HRID1413436

反应详情

EQUATION

反应方程式

HRID 1413436 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

7.5 ml of triethylamine were slowly introduced into 300 ml of phosphorous oxychloride cooled to 0° C., then were added 30 g of 5-ethoxycarbonyl 4-hydroxy 2-ethyl pyrimidine (VII) prepared in the preceding stage and the suspension was brought up to 40° C. under nitrogen scavenging. After dissolution, the phosphorous oxychloride was evaporated and the residue diluted in a mixture of water and chloroform. This was decanted, the chloroform phase was twice washed with water, dried on sodium sulfate and the solvent evaporated. The raw product obtained, after checking the purity by thin layer chromatography, was reacted in the following stage 3.

WORKUP

后处理

  1. customprepared in the preceding stage
  2. customwas brought up to 40° C. under nitrogen scavenging
  3. dissolutionAfter dissolution
  4. customthe phosphorous oxychloride was evaporated
  5. additionthe residue diluted in a mixture of water and chloroform
  6. customThis was decanted
  7. washthe chloroform phase was twice washed with water
  8. customdried on sodium sulfate
  9. customthe solvent evaporated