HRID840000

反应详情

EQUATION

反应方程式

HRID 840000 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

1.46 g of the 5-allyl-1,2,5,6-tetrahydro-2,2,6,6-tetramethyl-4-piperidinopyridine thus obtained were dissolved in a mixture of 3 ml of acetic acid, 1.5 g of sodium acetate and 3 ml of water, and the solution was allowed to stand overnight. To the solution were then added 6.0 g of sodium bicarbonate and 3 ml of concentrated aqueous ammonia; the solution was then extracted with hexane. The hexane extract was dried over magnesium sulphate and then treated with charcoal giving, after removal of the hexane, 0.91 g of 3-allyl-2,2,6,6-tetramethyl-4-piperidone. On thin layer chromatography using a 0.25 mm thick layer of alumina 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 having an Rf value of 0.70.

WORKUP

后处理

  1. extractionthe solution was then extracted with hexane
  2. extractionThe hexane extract
  3. dry with materialwas dried over magnesium sulphate
  4. additiontreated with charcoal giving
  5. customafter removal of the hexane, 0.91 g of 3-allyl-2,2,6,6-tetramethyl-4-piperidone
  6. additiona mixture of benzene, hexane, ethyl acetate and triethylamine (2 : 2 : 1 : 0.5 by volume)