HRID1380842
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
PROCEDURE
实验过程
A mixture of 6.5 g (0.036 mol) of 4-hydroxy-2-isopropyl-6-methyl-pyrimidine and 16.8 g (0.108 mol) of phosphorus oxychloride in 40 ml of chloroform is heated at reflux for 2 hours. The solution is then concentrated under reduced pressure, the residue is poured into water and the aqueous phase is extracted twice with 100 ml of n-hexane each time. The organic phase is dried over anhydrous sodium sulphate and subsequently evaporated. There is obtained 4-chloro-2-isopropyl-6-methyl-pyrimidine in the form of an orange oil, 1H-NMR (CDCl3): 1.32 (d, CH(CH3)2), 2.48 (s, CH3), 3.17 (m, CH(CH3)2), 7.03 (s, CH).
WORKUP
后处理
- temperatureis heated
- temperatureat reflux for 2 hours
- concentrationThe solution is then concentrated under reduced pressure
- additionthe residue is poured into water
- extractionthe aqueous phase is extracted twice with 100 ml of n-hexane each time
- dry with materialThe organic phase is dried over anhydrous sodium sulphate
- customsubsequently evaporated