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
2.2 g of the 1,2,5,6-tetrahydro-2,2,6,6-tetramethyl-4-piperidinopyridine and 1.2 g of allyl bromide were dissolved in 3 ml of chloroform and the solution was then allowed to stand at room temperature for 24 hours. The crystals which precipitated were filtered off, washed with hexane and dissolved in 4 ml of concentrated aqueous ammonia; the resulting solution was extracted with hexane. The hexane extract was dried over potassium carbonate and, after removal of the hexane, 1.3 g of 5-allyl-1,2,5,6-tetrahydro-2,2,6,6-tetramethyl-4-piperidinopyridine were obtained. On thin layer chromatography using a 0.25 mm thick layer of alumina ("60F 254", available from Merck & Co.) and a mixture of benzene, hexane, ethyl acetate and triethylamine (2 : 2 : 1 : 0.5 by volume) as developing solvent, the compound showed a single spot with an Rf value of 0.80.
WORKUP
后处理
- customThe crystals which precipitated
- filtrationwere filtered off
- washwashed with hexane
- dissolutiondissolved in 4 ml of concentrated aqueous ammonia
- extractionthe resulting solution was extracted with hexane
- extractionThe hexane extract
- dry with materialwas dried over potassium carbonate
- customafter removal of the hexane