تفاعل #62958

ord-30e2e597742e44bcb9f8d17534a43186

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONTo this mixture there is added at room temperature
  2. 2
    أخرىAn instantaneous exothermic reaction
  3. 3
    أخرى(40° C.)
  4. 4
    أخرىthe product crystallizes from the solution
  5. 5
    workup.WAITto stand overnight at room temperature
  6. 6
    ترشيحfiltered

الإجراء التجريبي

In the typical procedure, 0.1 mole of benzofurazan 1-oxide and 0.12 mole of nitroethane is dissolved at 100 ml. of tetrahydrofuran. To this mixture there is added at room temperature, 0.12 mole of diethylamine over a period of 0.5 hour. An instantaneous exothermic reaction is observed (40° C.) and within one hour, the product crystallizes from the solution. The solution is allowed to stand overnight at room temperature and filtered to yield 9.6 grams of 2-methyl-1-hydroxy-1-H-benzimidazole 3-oxide (Table I, Example 2). The product can be rectystallized from methanol.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04762870uspto-grants-1988_08