تفاعل #4674

ord-c4b9f4b95d474b5a9a51663bf3ff7ff1

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe dicyclohexylurea which precipitated
  2. 2
    أخرىwas removed by filtration
  3. 3
    أخرىthe solvent was removed by rotary evaporation
  4. 4
    أخرىThe crude product was recrystallized from ethyl acetate
  5. 5
    أخرىto give light yellow crystals which
  6. 6
    أخرىThe product, obtained in 72% yield (5.2 g) and melting at 129°-131° C.

الإجراء التجريبي

Nicotinic acid (4.025 g, 0.0327 mol) and N-hydroxysuccinimide (3.763 g, 0.0327 mol) were dissolved in 130 ml of dioxane. Dicyclohexylcarbodiimide (6.75 g, 0.032 mol) in 20 ml of dioxane was added. The reaction mixture was then stirred at room temperature for 3 hours. The dicyclohexylurea which precipitated was removed by filtration and the solvent was removed by rotary evaporation. The crude product was recrystallized from ethyl acetate to give light yellow crystals which were then waashed with anhydrous ether. The product, obtained in 72% yield (5.2 g) and melting at 129°-131° C., has the formula: ##STR40##

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04727079uspto-grants-1988_02