反应 #575030

反应方程式

dichloromethane

acid chloride

1-(4-chlorocarbonylbutyl)-5-ethyl-5-phenyl-2,4,6(1H,3H,5H)pyrimidinetrione

benzyl 1-piperazinecarboxylate

triethylamine

→

1-[4-(4-Benzyloxycarbonyl-1-piperazinylcarbonyl)butyl]-5-ethyl-5-phenyl-2,4,6(1H,3H,5H)pyrimidinetrione

溶剂

chloroform

chloroform

反应条件

后处理

1. 1
   洗涤The mixture was washed with 10% hydrochloric acid solution (3×100 mL)
2. 2
   洗涤washed with saturated sodium chloride solution (100 mL)
3. 3
   干燥dried over anhydrous magnesium sulfate
4. 4
   过滤filtered
5. 5
   其他the solvent removed
6. 6
   其他The residue was then chromatographed on SiO2
7. 7
   其他to give a solid

实验过程

The acid chloride of step 3 (0.2 mole) in chloroform (75 mL) was added dropwise over 15 minutes to a mixture of benzyl 1-piperazinecarboxylate (6.0 g, 0.030 mole) and triethylamine (4.0 g, 0.04 mole) in chloroform (100 mL). This mixture was stirred at room temperature for 20 hrs, and dichloromethane was then added (300 mL). The mixture was washed with 10% hydrochloric acid solution (3×100 mL), washed with saturated sodium chloride solution (100 mL), dried over anhydrous magnesium sulfate, filtered, and the solvent removed. The residue was then chromatographed on SiO2 to give a solid.

来源