تفاعل #736832

ord-ba65959a6a3e47ddaa5a7c2120f7f89b

الكواشف

لا شيء

ظروف التفاعل

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

المعالجة

  1. 1
    درجة الحرارةthe temperature being maintained at between 0° C. and 5° C
  2. 2
    workup.ADDITION1 hour after the addition
  3. 3
    أخرىthe expected product precipitates
  4. 4
    تجفيفAfter being dried hot in the presence of phosphorus pentoxide, it melts at 99° C. (literature 98° C.-100° C.)
  5. 5
    أخرىIt can optionally be recrystallized from 96° strength ethanol

الإجراء التجريبي

0.103 mol (17.2 g) of 4,5-methylenedioxy-1-nitrobenzene is added in small portions in the course of 15 minutes to a mixture, cooled to -5° C., consisting of 125 ml of nitric acid (d=1.50) and 125 ml of nitric acid (d=1.40), the temperature being maintained at between 0° C. and 5° C. 1 hour after the addition is complete, the reaction mixture is poured onto 1 kg of ice; the expected product precipitates. After being dried hot in the presence of phosphorus pentoxide, it melts at 99° C. (literature 98° C.-100° C.). It can optionally be recrystallized from 96° strength ethanol.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04740622uspto-grants-1988_04