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
- 180 °C
PROCEDURE
实验过程
A mixture of 7.5 g of 2-[4-(5-[propyloxy]-1-pentyl)phenyl]-5-(ethoxy)pyrimidine, 10 g of sodium hydroxide and 120 ml of diethylene glycol was heated at 180° C. for 8 hours. The reaction mixture was poured into 100 ml of water, acidified with concentrated hydrochloric acid, then extracted three times with 50 ml of diethyl ether each time. The combined organic phases were washed twice with 100 ml of concentrated sodium chloride solution, dried over magnesium sulfate, filtered and subsequently concentrated. Chromatography of the residue on silica gel with hexane/ethyl acetate (vol. 7:3) and recrystallization from ethyl alcohol gave 5.2 g of 2-[4-(5-[propyloxy]-1-pentyl)phenyl]-5-hydroxypyrimidine.
WORKUP
后处理
- extractionextracted three times with 50 ml of diethyl ether each time
- washThe combined organic phases were washed twice with 100 ml of concentrated sodium chloride solution
- dry with materialdried over magnesium sulfate
- filtrationfiltered
- concentrationsubsequently concentrated
- customChromatography of the residue on silica gel with hexane/ethyl acetate (vol. 7:3) and recrystallization from ethyl alcohol