反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionafter the addition
- extractionThe subsequent mixture was extracted into ethyl acetate (2×30 ml.)
- dry with materialthe combined extracts were dried (MgSO4)
- customevaporated
- dissolutionThe residue was dissolved in acetone (50 ml.)
- additionthe solution was treated with concentrated hydrochloric acid to pH2
- customThe solid which precipitated
- filtrationwas collected by filtration
- customrecrystallised from isopropanol