HRID337675
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
To a MeOH solution (0.2 M) of 1-(1,1-dimethylethyl) 3-ethyl 5,6-dihydro-4,4′-bipyridine-1,3(2H)-dicarboxylate (1 eq.) from the previous step was added magnesium turnings (3 eq.). The suspension was evacuated and back-filled with N2. Finally, the reaction mixture was sonicated at RT for 2 h during which the magnesium turnings disappeared. The reaction was then quenched with the addition of EtOAc and 1 N aq. NaOH. The aqueous layer was separated and back-extracted with EtOAc. The combined organic extracts were washed further with water and brine, dried over Na2SO4 and filtered. Concentration of the filtrate in vacuo afforded the title compound as a golden yellow oil.
WORKUP
后处理
- customThe suspension was evacuated
- additionback-filled with N2
- customFinally, the reaction mixture was sonicated at RT for 2 h during which the magnesium turnings
- customThe reaction was then quenched with the addition of EtOAc and 1 N aq. NaOH
- customThe aqueous layer was separated
- extractionback-extracted with EtOAc
- washThe combined organic extracts were washed further with water and brine
- dry with materialdried over Na2SO4
- filtrationfiltered