HRID1732922

反应详情

EQUATION

反应方程式

HRID 1732922 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

54.6 g 2,2,6,6-Tetramethyl-4-hydroxy-4-cyanopiperidine together with 45 g tert.-butanol in 200 ml glacial acetic acid are introduced into the reactor. Subsequently, 60 g concentrated sulfuric acid are added dropwise with agitation, and agitation is continued for 2 hours at 70° C., thus forming a precipitate which is filtered off and dissolved in water. On alkalization with NaOH, the product precipitates, it is suction-filtered and recrystallized from ethyl acetate. Yield 44 g, m.p. 134°-136° C.

WORKUP

后处理

  1. customthus forming a precipitate which
  2. filtrationis filtered off
  3. dissolutiondissolved in water
  4. customOn alkalization with NaOH, the product precipitates
  5. filtrationit is suction-filtered
  6. customrecrystallized from ethyl acetate