반응 #75115

반응 방정식

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

methylene chloride

chloroformic acid octyl ester

→

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

용매

triethylamine

반응 조건

후처리

1. 1
   온도The mixture is cooled for 30 minutes
2. 2
   workup.STIRRINGstirred at room temperature for 1 hour
3. 3
   추출The mixture is extracted with methylene chloride
4. 4
   세척washed with water
5. 5
   건조dried over magnesium sulfate
6. 6
   기타evaporated under reduced pressure
7. 7
   기타The residue is recrystallized from methylene chloride/ethanol, there

실험 절차

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.

출처