反应详情

2.2 of the 1,2,5,6-tetrahydro-2,2,6,6-tetramethyl-4-piperidinopyridine thus obtained and 1.2 g of allyl bromide were dissolved in 3 ml of chloroform and the solution was allowed to stand for 24 hours at room temperature. The crystals which precipitated were filtered off, washed with hexane and dissolved in 4 ml of concentrated aqueous ammonia; the solution was then extracted with hexane. The extract was dried over potassium carbonate and, after removing the hexane, 1.3 g of 5-allyl-1,2,5,6-tetrahydro-2,2,6,6-tetramethyl-4-piperidinopyridine were obtained. The compound showed a single spot on thin layer chromatography using a 0.25 mm thick layer of alumina (available from Merck & Co. under the trade name "60F 254") and using a mixture of benzene/hexane/ethyl acetate/triethylamine (2 : 2 1 : 0.5 by volume) s developing solvent; the Rf value was 0.80.

1. customThe crystals which precipitated
2. filtrationwere filtered off
3. washwashed with hexane
4. dissolutiondissolved in 4 ml of concentrated aqueous ammonia
5. extractionthe solution was then extracted with hexane
6. dry with materialThe extract was dried over potassium carbonate
7. customafter removing the hexane