HRID223577
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
A suspension of 4.0 g of 3-(4-piperidyl)-1,2-benzisoxazole, 2.6 g of allyl bromide, 5.0 g of sodium bicarbonate, and 3.0 g of potassium iodide in 90 ml of dimethylformamide was stirred at 80° for 20 hrs. The reaction was cooled, filtered and poured into 1 l of water. The mixture was extracted with ether (three times) and dried over anhydrous sodium sulfate. The solvent was removed under reduced pressure to give an oil. The oil was dissolved in a small amount of ether into which hydrochloric acid was bubbled. The precipitate was recrystallized from ethanol-ether (three times) to give 2.4 g of product, mp, 174°-176°.
WORKUP
后处理
- temperatureThe reaction was cooled
- filtrationfiltered
- additionpoured into 1 l of water
- extractionThe mixture was extracted with ether (three times)
- dry with materialdried over anhydrous sodium sulfate
- customThe solvent was removed under reduced pressure
- customto give an oil
- customwas bubbled
- customThe precipitate was recrystallized from ethanol-ether (three times)