反应 #1925198

ord-99afc5a35d364684ad00f4364911879e

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他A flask equipped with a stirrer
  2. 2
    温度under reflux for 4 hours
  3. 3
    workup.ADDITIONwere added to the reactant
  4. 4
    萃取to an acidity and effect ethyl acetate extraction
  5. 5
    洗涤The resulting organic phase was washed with NaCl saturated water
  6. 6
    干燥dried over anhydrous sodium sulfate
  7. 7
    过滤filtered
  8. 8
    浓缩concentrated

实验过程

A flask equipped with a stirrer and a thermometer was charged with 5.41 g (20.6 mmol) of 5-[4-(3-methyl-3-hydroxybutyne-1-yl)phenoxy]pentanol and 70 ml of toluene under a nitrogen atmosphere. To the flask, 1.65 g (41.2 mmol) of sodium hydroxide was added, and stirred under reflux for 4 hours. After the completion of the reaction, water, 1N hydrochloric acid, and ethyl acetate were added to the reactant to adjust the pH to an acidity and effect ethyl acetate extraction. The resulting organic phase was washed with NaCl saturated water, dried over anhydrous sodium sulfate, filtered, and concentrated to thereby obtain 4.13 g of 5-(4-ethynylphenoxy)pentanol in the form of a brown oil in a 98% yield.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06673267B2uspto-grants-2004_01