반응 #75116

ord-8a990e8610d14b2e90e8631959b728bb

반응 방정식

Nc1cc(N2CC=CCC2)nc(N)[n+]1[O-]
2,4-diamino-6-[3,6-dihydro-1(2H)-pyridyl]pyrimidine-3-oxide
ClCCl
methylene chloride
COCCOC(=O)Cl
chloroformic acid 2-methoxyethyl ester
COCCOC(=O)Nc1cc(N2CC=CCC2)nc(NC(=O)OCCOC)[n+]1[O-]
bis(2-methoxyethyl) 6-[3,6-dihydro-1(2H)-pyridyl]-2,4-pyrimidine-dicarbamate-3-oxide

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    세척washed with water
  2. 2
    추출extracted with methylene chloride
  3. 3
    기타The organic phases are evaporated under reduced pressure
  4. 4
    기타the residue is recrystallized from diethyl ether, there

실험 절차

10 G. of 2,4-diamino-6-[3,6-dihydro-1(2H)-pyridyl]pyrimidine-3-oxide are stirred at 5° C. in 150 ml. of methylene chloride and 30 ml. of triethylamine and treated with 20 ml. of chloroformic acid 2-methoxyethyl ester. The mixture is stirred at room temperature for 4 hours, then washed with water and extracted with methylene chloride. The organic phases are evaporated under reduced pressure and the residue is recrystallized from diethyl ether, there being obtained bis(2-methoxyethyl) 6-[3,6-dihydro-1(2H)-pyridyl]-2,4-pyrimidine-dicarbamate-3-oxide, having a melting point of 126°-128° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04175189uspto-grants-1979_11