HRID236572
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- concentrationThe mixture is concentrated
- concentrationthe concentrate is concentrated at 70° C.
- dissolutionthe residue is dissolved in chloroform
- washthe solution is washed twice with water
- customdried
- concentrationconcentrated
- customThe resulting evaporation residue
- customis purified over a silica gel column with a volume of 160 ml