反应详情

(±)-4-(4-Chlorophenyl)-2,3,9-trimethyl-6H-thieno[3,2-f][1,2,4]triazolo[4,3-a][1,4]diazepine-6-acetic acid (1.0 g), 2-aminopyrimidine (0.28 g) and pyridine (0.49 ml) are added to dichloroethane (15 ml), and the mixture is stirred in an ice bath. A solution of 2-chloro-1,3-dimethylimidazolium chloride (0.63 g) in dichloroethane (12 ml) is dropwise added to this mixture at a temperature of not more than 5° C. The mixture is stirred at room temperature overnight, and the reaction mixture is washed with water and dried over anhydrous magnesium sulfate. The solvent is distilled away and the residue is purified by column chromatography (chloroform:methanol=20:1) and recrystallized from ethanol to give 0.78 g of (±)-N-(2-pyrimidinyl)-4-(4-chlorophenyl)-2,3,9-trimethyl-6H-thieno[3,2-f][1,2,4]triazolo[4,3-a][1,4]diazepine-6-acetamide, melting point 251°-253° C.

1. stirringThe mixture is stirred at room temperature overnight
2. washthe reaction mixture is washed with water
3. dry with materialdried over anhydrous magnesium sulfate
4. distillationThe solvent is distilled away
5. customthe residue is purified by column chromatography (chloroform:methanol=20:1)
6. customrecrystallized from ethanol