反応 #4674

反応方程式

ether

Nicotinic acid

N-hydroxysuccinimide

Dicyclohexylcarbodiimide

→

N-Nicotinoyloxysuccinimide

収率 72.0%

溶媒

dioxane

dioxane

反応条件

後処理

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

実験手順

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##

出典