HRID1413436
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customprepared in the preceding stage
- customwas brought up to 40° C. under nitrogen scavenging
- dissolutionAfter dissolution
- customthe phosphorous oxychloride was evaporated
- additionthe residue diluted in a mixture of water and chloroform
- customThis was decanted
- washthe chloroform phase was twice washed with water
- customdried on sodium sulfate
- customthe solvent evaporated