反应详情

温度

5 °C

10 G. of 2,4-diamino-6-[3,6-dihydro-1(2H)-pyridyl]pyrimidine-3-oxide are suspended in 150 ml. of methylene chloride and 20 ml. of triethylamine. The suspension is cooled to 5° C. and 28 g. of chloroformic acid octyl ester are added dropwise while stirring. The mixture is cooled for 30 minutes and then stirred at room temperature for 1 hour. The mixture is extracted with methylene chloride, washed with water, dried over magnesium sulfate and evaporated under reduced pressure. The residue is recrystallized from methylene chloride/ethanol, there being obtained dioctyl 6-[3,6-dihydro-1(2H)-pyridyl]-2,4-pyrimidine-dicarbamate-3-oxide, having a melting point of 64° C.

1. temperatureThe mixture is cooled for 30 minutes
2. stirringstirred at room temperature for 1 hour
3. extractionThe mixture is extracted with methylene chloride
4. washwashed with water
5. dry with materialdried over magnesium sulfate
6. customevaporated under reduced pressure
7. customThe residue is recrystallized from methylene chloride/ethanol, there