HRID260213

反应详情

EQUATION

反应方程式

HRID 260213 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

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 tool 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 washed with anhydrous ether. The product, obtained in 72% yield (5.2 g) and melting at 129°-131° C., has the formula: ##STR1535##

WORKUP

后处理

  1. customThe dicyclohexylurea which precipitated
  2. customwas removed by filtration
  3. customthe solvent was removed by rotary evaporation
  4. customThe crude product was recrystallized from ethyl acetate
  5. customto give light yellow crystals which
  6. washwere then washed with anhydrous ether
  7. customThe product, obtained in 72% yield (5.2 g) and melting at 129°-131° C.