HRID597549

反应详情

EQUATION

反应方程式

HRID 597549 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 78.5 parts of 2,2,6,6-tetramethylpiperidine-4-ol and 30.25 parts of allyl bromide in 250 parts of ethyl alcohol was heated under reflux conditions for 48 hours. The cooled reaction mixture was filtered to remove 2,2,6,6-tetramethylpiperidin-4-ol hydrobromide formed during the reaction and the ethyl alcohol solvent was removed by distillation under reduced pressure. The residue was triturated with cold petroleum ether (b.p. 40°-60°C) to remove a small amount of unreacted 2,2,6,6-tetramethylpiperidin-4-ol. Crystallisation of the residue from 40°-60°C petroleum ether gave 1-allyl-2,2,6,6-tetramethylpiperidin-4-ol having a melting point of 84°-5°C and the following elemental analysis by weight.

WORKUP

后处理

  1. temperaturewas heated under reflux conditions for 48 hours
  2. customThe cooled reaction mixture
  3. filtrationwas filtered
  4. customto remove 2,2,6,6-tetramethylpiperidin-4-ol hydrobromide
  5. customformed during the reaction
  6. customthe ethyl alcohol solvent was removed by distillation under reduced pressure
  7. customThe residue was triturated with cold petroleum ether (b.p. 40°-60°C)
  8. customto remove a small amount of unreacted 2,2,6,6-tetramethylpiperidin-4-ol
  9. customCrystallisation of the residue from 40°-60°C petroleum ether