تفاعل #80282

ord-c317843f65ba47bebddd862b2745b9a7

ظروف التفاعل

درجة الحرارة
70°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwas heated
  2. 2
    أخرىwas returned to room temperature
  3. 3
    استخلاصextracted with ethyl acetate
  4. 4
    غسيلThe organic layer was washed with water
  5. 5
    تجفيفdried over anhydrous magnesium sulfate
  6. 6
    أخرىCrystals obtained by concentration under reduced pressure
  7. 7
    غسيلwere washed with isopropyl ether

الإجراء التجريبي

A mixture comprising 54.2 g of 4-allyloxycarbonyl-5-hydroxy-2-methylbenzofuran-3-carboxylic acid, 47 g of 4,6-dimethoxy-2-methylsulfonylpyridine and 65 g of potassium carbonate in 200 ml of N,N-dimethylformamide, was heated and stirred at 70° C. for two hours. The mixture was returned to room temperature, and then the reaction solution was poured into water and extracted with ethyl acetate. The organic layer was washed with water and then dried over anhydrous magnesium sulfate. Crystals obtained by concentration under reduced pressure, were washed with isopropyl ether to obtain 79.2 g (yield: 98%) of the desired compound.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05616537uspto-grants-1997_04