反応 #347395
ord-c76525e3de3b438688e8aeca2a8ef39b
反応条件
詳細条件
See reaction.notes.procedure_details.
後処理
- 1その他The dicyclohexylurea which precipitated
- 2その他was removed by filtration
- 3その他the solvent was removed by rotary evaporation
- 4その他The crude product was recrystallized from ethyl acetate
- 5その他to give light yellow crystals which
- 6洗浄were then washed with anhydrous ether
- 7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 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##