반응 #75111

반응 방정식

2,4-diamino-6-[3,6-dihydro-1(2H)-pyridyl]pyrimidine-3-oxide

methylene chloride

chloroformic acid methyl ester

→

dimethyl 6-[3,6-dihydro-1(2H)-pyridyl]-2,4-pyrimidine-dicarbamate-3-oxide

용매

triethylamine

반응 조건

후처리

1. 1
   workup.STIRRINGThe mixture is stirred at 5° C. for 30 minutes and at room temperature for 18 hours
2. 2
   workup.ADDITIONThen, the mixture is treated with 100 ml
3. 3
   추출of methanol and subsequently extracted with 400 ml
4. 4
   세척of methylene chloride, washed with water
5. 5
   건조dried over potassium carbonate
6. 6
   기타evaporated under reduced pressure
7. 7
   기타Recrystallization of the residue from methanol

실험 절차

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 at 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.

출처