反応 #54723

ord-e692b1acb2a5489b9ba6844e903683e5

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    洗浄washed with water
  2. 2
    抽出extracted with methylene chloride
  3. 3
    その他The organic phases are evaporated under reduced pressure
  4. 4
    その他the residue is recrystallized from diethyl ether, there

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04150132uspto-grants-1979_04