反应详情

3.40 g (50 millimoles) of imidazole are dissolved in 25 ml of absolute tetrahydrofuran, a solution of 3.54 g (25 millimoles) of nicotinoyl chloride in 25 ml of absolute tetrahydrofuran is added dropwise at room temperature, and the mixture is stirred for a further 2 hours. The imidazole hydrochloride which has precipitated is then filtered off, the filter residue is washed with a small amount of anhydrous tetrahydrofuran, the combined filtrates are added to a solution of 4.6 g (20 millimoles) of 2-(2',6'-dichlorophenylamino)-2-imidazoline in 25 ml of absolute tetrahydrofuran, and the mixture is stirred overnight. The solvent is then stripped off under reduced pressure on a rotary evaporator and the residue is twice recrystallized from isopropanol. 4.8 g of pure 1-nicotinoyl-2-(2',6'-dichlorophenylamino)-2-imidazoline of melting point 172.5°-174° C. are obtained; the material is identical with the product described in Example 1.

1. customThe imidazole hydrochloride which has precipitated
2. filtrationis then filtered off
3. washthe filter residue is washed with a small amount of anhydrous tetrahydrofuran
4. stirringthe mixture is stirred overnight
5. customThe solvent is then stripped off under reduced pressure on a rotary evaporator
6. customthe residue is twice recrystallized from isopropanol