反应详情

A mixture of 2-chloro-4-(3-chloro-4-methoxybenzylamino)-5-ethoxycarbonylpyrimidine (prepared in Example 95) 285 mg, 5,6,7,8-tetrahydroimidazo[1,2-a]pyrazine 197 mg, triethylamine 0.22 ml and chloroform 3 ml is stirred at room temperature for 2.5 hours, followed by stirring at 60° C. for 2.5 hours. The mixture is diluted with ethyl acetate, and washed with water. The water layer is extracted with ethyl acetate, and the organic layer is washed with water and an aqueous saturated sodium chloride solution, dried over anhydrous sodium sulfate and concentrated in vacuo. The residue is purified with silica gel chromatography (silica gel 10 g, solvent; chloroform:methanol=50:1) and concentrated in vacuo and triturated with isopropyl ether to give 2-(5,6,7,8-tetrahydroimidazo[1,2-a]pyrazin-7-yl)-4-(3-chloro-4-methoxybenzylamino)-5-ethoxycarbonylpyrimidine as a colorless crystalline powder, 290 mg. mp 179-182° C., MS(m/z): 443(M+H)+

1. stirringby stirring at 60° C. for 2.5 hours
2. washwashed with water
3. extractionThe water layer is extracted with ethyl acetate
4. washthe organic layer is washed with water
5. dry with materialan aqueous saturated sodium chloride solution, dried over anhydrous sodium sulfate
6. concentrationconcentrated in vacuo
7. customThe residue is purified with silica gel chromatography (silica gel 10 g, solvent; chloroform:methanol=50:1)
8. concentrationconcentrated in vacuo
9. customtriturated with isopropyl ether