HRID32336

反应详情

EQUATION

反应方程式

HRID 32336 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customthe insoluble dicyclohexylurea removed by filtration
  2. customThe solvent was removed by rotary evaporation
  3. dissolutionthe residue dissolved in 30-40 mL CH2Cl2
  4. additionApproximately 10 mL hexane was added
  5. additionAdditional hexane was added dropwise until small planar white crystals
  6. customto form
  7. waitthe solution was refrigerated overnight
  8. washwashed with hexane
  9. customdried in vacuum (2.30 g, 70.0%)