HRID64586
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
To a solution of NaOH (0.8 g, 0.02 mol) dissolved in dry methanol (30 ml) were added 2-(p-pentylphenyl)-5-pyrimidinecarboxamidine hydrochloride (3.0 g, 0.01 mol) and α-propyl -β-dimethylaminoacrolein (1.4 g, 0.01 mol), followed by boiling with stirring for 2 hours and then distilling off methanol. Water (100 ml) and toluene (100 ml) were added to the reaction residue to extract the product, followed by washing the extraction liquor with water, drying the toluene layer over anhydrous sodium sulfate, distilling off toluene and three times recrystallizing the residual solids from ethanol to obtain the objective 2-(p-pentylphenyl)-5'-propyl-5,2'-bipyrimidinyl (2.0 g, 0.006 mol).
WORKUP
后处理
- distillationdistilling off methanol
- additionWater (100 ml) and toluene (100 ml) were added to the reaction residue
- extractionto extract the product
- washby washing the extraction liquor with water
- dry with materialdrying the toluene layer over anhydrous sodium sulfate
- distillationdistilling off toluene and three times
- customrecrystallizing the residual solids from ethanol