HRID345177

反应详情

EQUATION

反应方程式

HRID 345177 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 25 ml of dichloromethane, were dissolved 5.0 g (41.3 mmol) of benzaldoxime and 4.5 g (45.9 mmol) of 1-hexyne-3-ol. Under ice cooling, 29.0 g of a 12.0% aqueous solution of sodium hypochlorite were added dropwise to the solution over 30 minutes. After completion of the dropwise addition, they were reacted at 20° C. for 2 hours. After completion of the reaction, the reaction mixture was extracted with dichloromethane and the organic layer was washed with water. The organic layer was dried over anhydrous sodium sulfate and the solvent was then distilled off under reduced pressure. The residue was purified by chromatography on a silica gel column (eluent: chloroform), whereby the target compound, namely, 5-(1-hydroxybutyl)-3-phenylisooxazole was obtained as an oil.

WORKUP

后处理

  1. additionAfter completion of the dropwise addition, they
  2. customwere reacted at 20° C. for 2 hours
  3. customAfter completion of the reaction
  4. extractionthe reaction mixture was extracted with dichloromethane
  5. washthe organic layer was washed with water
  6. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  7. distillationthe solvent was then distilled off under reduced pressure
  8. customThe residue was purified by chromatography on a silica gel column (eluent: chloroform), whereby the target compound