HRID236554

反应详情

EQUATION

反应方程式

HRID 236554 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Benzoyl chloride (3.0 g.) was added to a vigorously stirred mixture of 1-(4-hydroxybenzyl)-1,2,3,6-tetrahydropyridine (4.0 g.) in N-sodium hydroxide solution (22 ml.) and ether (30 ml.). The mixture was stirred for 2 hours after the addition and then 3N-sodium hydroxide solution added to pH10. The subsequent mixture was extracted into ethyl acetate (2×30 ml.) and the combined extracts were dried (MgSO4) and evaporated. The residue was dissolved in acetone (50 ml.) and the solution was treated with concentrated hydrochloric acid to pH2. The solid which precipitated was collected by filtration and recrystallised from isopropanol to give 1-(4-benzoyloxybenzyl)-1,2,3,6-tetrahydropyridine (1.8 g.), m.p. 220°-227° C.

WORKUP

后处理

  1. additionafter the addition
  2. extractionThe subsequent mixture was extracted into ethyl acetate (2×30 ml.)
  3. dry with materialthe combined extracts were dried (MgSO4)
  4. customevaporated
  5. dissolutionThe residue was dissolved in acetone (50 ml.)
  6. additionthe solution was treated with concentrated hydrochloric acid to pH2
  7. customThe solid which precipitated
  8. filtrationwas collected by filtration
  9. customrecrystallised from isopropanol