反应 #6244

反应方程式

4-hydroxypyridine

N-(2-bromoethyl)phthalimide

1,8-diazabicyclo[5.4.0]-7-undecene

→

desired compound

收率 3.1%

4-(2-phthalimidoethyloxy)pyridine

收率 3.1%

溶剂

DMF

反应条件

后处理

1. 1
   workup.DISTILLATIONAfter the solvent was distilled off
2. 2
   workup.ADDITIONthe mixture was poured into water
3. 3
   萃取extracted with ethyl acetate
4. 4
   洗涤The mixture was washed with water
5. 5
   干燥dried over anhydrous magnesium sulfate
6. 6
   workup.DISTILLATIONthe solvent was distilled off
7. 7
   其他The residue was purified by column chromatography (eluent: ethyl acetate)

实验过程

To a solution of 4.76 g (50 mmol) of 4-hydroxypyridine and 13.97 g (55 mmol) of N-(2-bromoethyl)phthalimide in 80 ml of DMF, 8.23 ml (55 mmol) of 1,8-diazabicyclo[5.4.0]-7-undecene was added. The mixture was stirred at room temperature for 32 hours. After the solvent was distilled off, the mixture was poured into water and extracted with ethyl acetate. The mixture was washed with water and dried over anhydrous magnesium sulfate, and then the solvent was distilled off. The residue was purified by column chromatography (eluent: ethyl acetate) to obtain 0.41 g of the desired compound (yield: 3.1%, colorless crystal).

来源