تفاعل #44421

ord-6114b1af78d34b06bd69b96fd94d0f90

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىdoes not exceed 5° C
  2. 2
    درجة الحرارةunder reflux for 5 h
  3. 3
    درجة الحرارةafter it has cooled down
  4. 4
    workup.ADDITIONpoured onto ice
  5. 5
    استخلاصThe product is extracted with ethyl acetate (3×100 ml)
  6. 6
    أخرىdried (Na2 SO4)
  7. 7
    ترشيحThe mixture is filtered
  8. 8
    workup.DISTILLATIONthe solvent is distilled off in vacuo

الإجراء التجريبي

Phosphoryl chloride (55 ml) is carefully added to barbituric acid (10 g, 78.1 mmol) at 0° C. Water (1.7 ml) is then added dropwise such that the temperature does not exceed 5° C. The mixture is boiled under reflux for 5 h and, after it has cooled down, poured onto ice. The product is extracted with ethyl acetate (3×100 ml) and dried (Na2 SO4). The mixture is filtered and the solvent is distilled off in vacuo.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07737144B2uspto-grants-2010_06