HRID337675

反应详情

EQUATION

反应方程式

HRID 337675 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe suspension was evacuated
  2. additionback-filled with N2
  3. customFinally, the reaction mixture was sonicated at RT for 2 h during which the magnesium turnings
  4. customThe reaction was then quenched with the addition of EtOAc and 1 N aq. NaOH
  5. customThe aqueous layer was separated
  6. extractionback-extracted with EtOAc
  7. washThe combined organic extracts were washed further with water and brine
  8. dry with materialdried over Na2SO4
  9. filtrationfiltered