반응 #4674

반응 방정식

ether

Nicotinic acid

N-hydroxysuccinimide

Dicyclohexylcarbodiimide

→

N-Nicotinoyloxysuccinimide

수율 72.0%

용매

dioxane

dioxane

반응 조건

후처리

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

실험 절차

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##

출처