تفاعل #75114

ord-bef6d215d3864614beb53eb650a756f1

المذيبات

ظروف التفاعل

درجة الحرارة
5°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONThe mixture is treated with 45 ml
  2. 2
    أخرىThe mixture obtained
  3. 3
    غسيلis washed with water
  4. 4
    استخلاصextracted with methylene chloride
  5. 5
    أخرىevaporated under reduced pressure
  6. 6
    أخرىThe residue is recrystallized from ethanol, there

الإجراء التجريبي

20 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, stirred and cooled to 5° C. The mixture is treated with 45 ml. of chloroformic acid butyl ester and stirred at room temperature for 6 hours. The mixture obtained is washed with water, extracted with methylene chloride and evaporated under reduced pressure. The residue is recrystallized from ethanol, there being obtained dibutyl 6-[3,6-dihydro-1(2H)-pyridyl]-2,4-pyrimidine-dicarbamate-3-oxide, having a melting point of 131°-132° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04175189uspto-grants-1979_11