HRID1914728

反应详情

EQUATION

反应方程式

HRID 1914728 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

30 g (0.125 mol) of ethyl (3-ethoxy-2-oxocyclohex-3-en-1-yl)(oxo)acetate were dissolved in 150 mL of glacial acetic acid and 6.5 mL of methylhydrazine (0.125 mol) were added. The mixture was stirred at room temperature for 6 hours. The solvent was then evaporated and the crude redissolved in water, made basic with 30% NH4OH and extracted with dichlormethane. The organic layer was then dried over Na2SO4 and concentrated. The residue was crystallized from diethyl ether to give 19.2 g (68% yield) of title compound.

WORKUP

后处理

  1. customThe solvent was then evaporated
  2. dissolutionthe crude redissolved in water
  3. extractionextracted with dichlormethane
  4. dry with materialThe organic layer was then dried over Na2SO4
  5. concentrationconcentrated
  6. customThe residue was crystallized from diethyl ether