HRID1288026

反应详情

EQUATION

反应方程式

HRID 1288026 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 6.2 g. of 1-methyl-2-nitro-5-vinylimidazole in 570 ml. of ethanol cooled to about -10° C., a solution of 5.46 g. of KMnO4 and 8.85 g. of MgSO4.7H2O in 750 ml. of H2O is added with stirring. The reaction mixture is filtered through Celite and washed with ethanol. The filtrate is concentrated to dryness under vacuum at 50° C., and the residue is taken up with acetone. The resulting solution is filtered and concentrated to dryness under vacuum. The resulting solid is crystallized from methyl ethyl ketone. Yield 3.15 g. (41.6%), m.p. 119°-121° C.

WORKUP

后处理

  1. filtrationThe reaction mixture is filtered through Celite
  2. washwashed with ethanol
  3. concentrationThe filtrate is concentrated to dryness under vacuum at 50° C.
  4. filtrationThe resulting solution is filtered
  5. concentrationconcentrated to dryness under vacuum
  6. customThe resulting solid is crystallized from methyl ethyl ketone