HRID236572

反应详情

EQUATION

反应方程式

HRID 236572 的结构方程式

PROCEDURE

实验过程

3 g of 1,4-dihydro-2,6-dimethyl-3-nitro-4-(2-chlorophenyl)-pyridine-5-carboxylic acid imidazolide are boiled in 12.5 ml of absolute tetrahydrofuran with 5 ml of mercaptoethanol for 7 hours. The mixture is concentrated, the concentrate is concentrated at 70° C. using an oil pump, the residue is dissolved in chloroform and the solution is washed twice with water, dried and concentrated. The resulting evaporation residue is purified over a silica gel column with a volume of 160 ml, using toluene and later toluene/ethyl acetate 6:1 as the mobile phase. 1.94 g of a yellow foam with an Rf value of 0.25 are obtained as the main fraction.

WORKUP

后处理

  1. concentrationThe mixture is concentrated
  2. concentrationthe concentrate is concentrated at 70° C.
  3. dissolutionthe residue is dissolved in chloroform
  4. washthe solution is washed twice with water
  5. customdried
  6. concentrationconcentrated
  7. customThe resulting evaporation residue
  8. customis purified over a silica gel column with a volume of 160 ml