تفاعل #6244

معادلة التفاعل

4-hydroxypyridine

N-(2-bromoethyl)phthalimide

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

→

desired compound

المردود 3.1%

4-(2-phthalimidoethyloxy)pyridine

المردود 3.1%

المذيبات

DMF

ظروف التفاعل

المعالجة

1. 1
   workup.DISTILLATIONAfter the solvent was distilled off
2. 2
   workup.ADDITIONthe mixture was poured into water
3. 3
   استخلاصextracted with ethyl acetate
4. 4
   غسيلThe mixture was washed with water
5. 5
   تجفيفdried over anhydrous magnesium sulfate
6. 6
   workup.DISTILLATIONthe solvent was distilled off
7. 7
   أخرىThe residue was purified by column chromatography (eluent: ethyl acetate)

الإجراء التجريبي

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).

المصدر