HRID653781

反应详情

EQUATION

反应方程式

HRID 653781 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 14.6 g of 4-methyl-1-(3-nitrophenyl)-1H-imidazole, 766 mg of palladium black, 19.6 g of sodium formate, 12.8 ml of formic acid in 300 ml of methyl alcohol is stirred for 18 hours under a hydrogen atmosphere. The mixture is filtered through diatomaceous earth and the filtrate evaporated to a residue. The residue is partitioned between saturated potassium bicarbonate and chloroform. The organic layer is dried and evaporated to a residue which is dissolved in a minimum of chloroform and passed through a pad of hydrous magnesium silicate. The filtrate is evaporated to a residue which is stirred with ether and the resulting solid filtered and air dried to give 10.3 g of the desired product as a solid, m.p. 117°-119° C.

WORKUP

后处理

  1. filtrationThe mixture is filtered through diatomaceous earth
  2. customthe filtrate evaporated to a residue
  3. customThe residue is partitioned between saturated potassium bicarbonate and chloroform
  4. customThe organic layer is dried
  5. customevaporated to a residue which
  6. dissolutionis dissolved in a minimum of chloroform
  7. customThe filtrate is evaporated to a residue which
  8. stirringis stirred with ether
  9. filtrationthe resulting solid filtered
  10. customair dried