تفاعل #170703

ord-229ae9931b90416da53922cb27a1b3f5

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
30°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىa temperature of the reaction solution below 45° C.
  2. 2
    درجة الحرارةthe mixture was heated to 55° C
  3. 3
    workup.STIRRINGthe mixture was stirred for 20 minutes
  4. 4
    workup.STIRRINGstirred for 1 hour
  5. 5
    ترشيحThe precipitated solid was collected by filtration
  6. 6
    غسيلwashed with cold water and ethanol
  7. 7
    أخرىdried under reduced pressure

الإجراء التجريبي

To a solution of itaconic acid (26.0 g) in water (35 ml) was added dropwise bromine (10.3 ml) at room temperature while keeping a temperature of the reaction solution below 45° C., and then the mixture was stirred at 30° C. for 15 minutes. To this reaction solution was added portionwise sodium hydrogen carbonate (33.6 g), and then the mixture was heated to 55° C. To this reaction solution was added dropwise a solution of sodium carbonate (10.6 g) in water (15 ml), and then the mixture was stirred for 20 minutes. This reaction solution was iced, and stirred for 1 hour. The precipitated solid was collected by filtration, washed with cold water and ethanol, and then dried under reduced pressure to give the titled compound (16.8 g).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08846746B2uspto-grants-2014_09