تفاعل #1483127

ord-f52ddab1220c46e681b072bfc172c293

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
120°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe mixture was heated
  2. 2
    أخرىto remove water
  3. 3
    أخرىgenerated during the reaction
  4. 4
    أخرىthe reactant kept being reacted
  5. 5
    درجة الحرارةthe reactant was cooled down
  6. 6
    أخرىproducing crystals
  7. 7
    ترشيحThe crystals were filtered
  8. 8
    أخرىonce more recrystallized

الإجراء التجريبي

342 mg of squaric acid and 2.12 g of 2-(methyl(3-acryloxyphenyl)amino)ethan-1-ol were put in a 100 mL 3-necked round bottom flask, and 40 mL of n-BuOH and 20 mL of toluene were added thereto. The mixture was heated and refluxed at 120° C. for 7 hours. Next, a Dean-Stark trap set was used to remove water generated during the reaction, and the reactant kept being reacted. When the reaction was complete, the reactant was cooled down, producing crystals. The crystals were filtered, several times cleaned with hexane, and once more recrystallized, obtaining a desired compound.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08900780B2uspto-grants-2014_12