反应详情

温度

50 °C

1 g of 1,5-dimethyl-2-nitroiminohexahydro-1,3,5-triazine was dissolved in 20 ml of dried DMF. To the solution, 0.27 g of 60% sodium hydride was added with cooling. The mixture was stirred for 1 hour at room temperature until evolution of hydrogen was ceased and then the mixture was heated with stirring further for 1 hour at 50° C. To the mixture, a solution of 0.9 g of 2-chloro-5-pyridylmethylchloride in 8 ml of dried DMF was added dropwise at 40-50° C. After this addition, the reaction mixture was heated with stirring it for two hours at 70-80° C. The mixture was poured into ice-water and extracted with dichloromethane. The extract was dried over anhydrous magnesium sulfate, and dichloromethane was distilled off. The residue was purified by a column chromatography to obtain 1.3 g of the title compound. This compound is No.5 in Table 1. m.p.: 116-117° C.

1. temperaturewith cooling
2. temperaturethe mixture was heated
3. additionAfter this addition
4. temperaturethe reaction mixture was heated
5. stirringwith stirring it for two hours at 70-80° C
6. extractionextracted with dichloromethane
7. dry with materialThe extract was dried over anhydrous magnesium sulfate, and dichloromethane
8. distillationwas distilled off
9. customThe residue was purified by a column chromatography