反应详情

温度

80 °C

A mixture of 2-hydroxy-4-(3-chloro-4-methoxybenzylamino)-5-ethoxycarbonylpyrimidine (prepared in Example 92) 500 mg, diethylaniline 2 ml and phosphoryl chloride 4 ml is stirred at 80° C. for 30 minutes and then at 100° C. for 5 hours. After cooling, the reaction solution is poured into water in ice and the mixture is stirred at room temperature for 30 minutes. The product 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 by silica gel chromatography (silica gel 7 g, solvent; chloroform) to give 2-chloro-4-(3-chloro-4-methoxybenzylamino)-5-ethoxycarbonylpyrimidine as a slightly yellow crystalline powder, 375 mg. mp 114–115° C. MS(m/z): 356(M+H)+

1. waitat 100° C. for 5 hours
2. temperatureAfter cooling
3. stirringthe mixture is stirred at room temperature for 30 minutes
4. extractionThe product is extracted with ethyl acetate
5. washthe organic layer is washed with water
6. dry with materialan aqueous saturated sodium chloride solution, dried over anhydrous sodium sulfate
7. concentrationconcentrated in vacuo
8. customThe residue is purified by silica gel chromatography (silica gel 7 g, solvent; chloroform)