反应 #4674

反应方程式

ether

Nicotinic acid

N-hydroxysuccinimide

Dicyclohexylcarbodiimide

→

N-Nicotinoyloxysuccinimide

收率 72.0%

溶剂

dioxane

dioxane

反应条件

后处理

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

实验过程

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##

来源