HRID839999

反应详情

EQUATION

反应方程式

HRID 839999 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

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