HRID32336
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 4 °C
PROCEDURE
实验过程
To Naproxen (2.303 g, 10 mmol) in 5 mL of dioxane was added N-hydroxysuccinimide (1.16 g, 10 mmol) dissolved in 15 mL of dioxane and dicyclohexylcarbodiimide (2.27 g, 11 mmol) in 25 mL of dioxane. The reaction was stirred overnight and the insoluble dicyclohexylurea removed by filtration. The solvent was removed by rotary evaporation and the residue dissolved in 30-40 mL CH2Cl2. Approximately 10 mL hexane was added and the mixture was chilled to 4° C. for 2 hr. Additional hexane was added dropwise until small planar white crystals began to form and the solution was refrigerated overnight. The activated ester was harvested, washed with hexane and dried in vacuum (2.30 g, 70.0%)
WORKUP
后处理
- customthe insoluble dicyclohexylurea removed by filtration
- customThe solvent was removed by rotary evaporation
- dissolutionthe residue dissolved in 30-40 mL CH2Cl2
- additionApproximately 10 mL hexane was added
- additionAdditional hexane was added dropwise until small planar white crystals
- customto form
- waitthe solution was refrigerated overnight
- washwashed with hexane
- customdried in vacuum (2.30 g, 70.0%)