反应详情

45 G. of 2,4-diamino-6-[3,6-dihydro-1(2H)-pyridyl]pyrimidine-3-oxide are mixed in 600 ml. of methylene chloride with 90 ml. of triethylamine and cooled to 5° C. 90 Ml. of chloroformic acid methyl ester are added dropwise while stirring. The mixture is stirred a 5° C. for 30 minutes and at room temperature for 18 hours. Then, the mixture is treated with 100 ml. of methanol and subsequently extracted with 400 ml. of methylene chloride, washed with water, dried over potassium carbonate and evaporated under reduced pressure. Recrystallization of the residue from methanol yields dimethyl 6-[3,6-dihydro-1(2H)-pyridyl]-2,4-pyrimidine-dicarbamate-3-oxide, having a melting point of 202°-203° C.

1. stirringThe mixture is stirred a 5° C. for 30 minutes and at room temperature for 18 hours
2. additionThen, the mixture is treated with 100 ml
3. extractionof methanol and subsequently extracted with 400 ml
4. washof methylene chloride, washed with water
5. dry with materialdried over potassium carbonate
6. customevaporated under reduced pressure
7. customRecrystallization of the residue from methanol