반응 #2139258

반응 방정식

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

methylene chloride

chloroformic acid isobutyl ester

→

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

용매

triethylamine

반응 조건

후처리

1. 1
   workup.ADDITIONAfter completion of the addition
2. 2
   workup.STIRRINGthe mixture is stirred at 50° C. for 15 minutes
3. 3
   workup.ADDITIONThe solution is treated with 200 ml
4. 4
   추출of water and extracted with methylene chloride
5. 5
   기타The organic phase is evaporated
6. 6
   기타the residue is crystallized from ethanol

실험 절차

20.7 G. of 2,4-diamino-6-[3,6-dihydro-1(2H)-pyridyl]pyrimidine-3-oxide are mixed with 250 ml. of methylene chloride and 35 ml. of triethylamine and cooled to 5° C. 40 Ml. of chloroformic acid isobutyl ester are added dropwise while stirring. After completion of the addition, the mixture is stirred at 50° C. for 15 minutes and then at room temperature for 2 hours. The solution is treated with 200 ml. of water and extracted with methylene chloride. The organic phase is evaporated and the residue is crystallized from ethanol. There is obtained diisobutyl 6-[3,6-dihydro-1(2H)-pyridyl]-2,4-pyrimidine-dicarbamate-3-oxide, having a melting point of 137°-139° C. (decomposition).

출처