反应详情

To a suspension of 40 mg of sodium hydride in 2 ml of N,N-dimethylformamide was added 0.22 g of 5-[(4-nitrophenyl)amino]pyrimidine in small portions. After stirring at room temperature for 30 minutes, 0.24 g of 4-trifluoromethylbenzyl bromide was added thereto, followed by stirring at room temperature for 2 hours. The solvent was distilled off under reduced pressure, water was added to the residue, and the mixture was extracted with chloroform. The chloroform layer was washed with water and dried over anhydrous magnesium sulfate. The solvent was distilled off, and the residue was purified by silica gel column chromatography to recover crude crystals from the chloroform eluate. Recrystallization of the crude crystals from a mixed solvent of ethyl acetate and ethyl ether yielded 0.19 g of 5-[N-(4-nitrophenyl)-N-(4trifluoromethylbenzyl)amino]pyrimidine.

1. stirringby stirring at room temperature for 2 hours
2. distillationThe solvent was distilled off under reduced pressure, water
3. additionwas added to the residue
4. extractionthe mixture was extracted with chloroform
5. washThe chloroform layer was washed with water
6. dry with materialdried over anhydrous magnesium sulfate
7. distillationThe solvent was distilled off
8. customthe residue was purified by silica gel column chromatography
9. customto recover crude crystals from the chloroform eluate
10. customRecrystallization of the crude crystals from a mixed solvent of ethyl acetate and ethyl ether