HRID236557

反应详情

EQUATION

反应方程式

HRID 236557 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

Triethylamine (1.2 g.) was added with stirring to a solution of 1-(4-hydroxybenzyl)-1,2,3,6-tetrahydropyridine (1.9 g.) in methylene chloride (30 ml.) at 0° C. Ethyl chloroformate (1.2 g.) was then added dropwise and the mixture stirred at 25° C. for 16 hours and then evaporated. Water (30 ml.) was added to the residue and the mixture was extracted with ether (2×30 ml.). The combined extracts were dried (MgSO4) and evaporated. The residue was dissolved in acetone (20 ml.) and acidified with ethereal hydrogen chloride to give 1-[4-(ethoxycarbonyloxy)benzyl]-1,2,3,6-tetrahydropyridine hydrochloride (1.5 g.) m.p. 168°-172° C. (after recrystallisation from ethanol-ethyl acetate).

WORKUP

后处理

  1. customevaporated
  2. additionWater (30 ml.) was added to the residue
  3. extractionthe mixture was extracted with ether (2×30 ml.)
  4. dry with materialThe combined extracts were dried (MgSO4)
  5. customevaporated
  6. dissolutionThe residue was dissolved in acetone (20 ml.)