反応 #343978

ord-455d0015f18a471f8d6cd93cf4c68d19

溶媒

反応条件

温度
140°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他water was collected as the reaction
  2. 2
    洗浄by washing three times with 50 ml saturated sodium bicarbonate solution
  3. 3
    その他The organic layer was collected
  4. 4
    乾燥dried over magnesium sulfate
  5. 5
    その他Excess decyl alcohol was removed by high vacuum distillation

実験手順

A 100 ml one neck round bottom flask equipped with a Dean Stark trap, condenser and nitrogen inlet/outlet was charged with 20.8 g (0.20 moles) 3-hydroxybutyric acid, 63.3 g (0.40 moles) decyl alcohol, and 0.1 g sulfuric acid (based on 0.5 g/mole 3-hydroxybutyric acid). The mixture was heated to 140° C. for 8 hours and water was collected as the reaction proceeded. The acid was neutralized by washing three times with 50 ml saturated sodium bicarbonate solution. Approximately 50 ml ether was needed to break the emulsion. The organic layer was collected and dried over magnesium sulfate. Excess decyl alcohol was removed by high vacuum distillation to yield 28.3 g (58% yield) of clear viscous colorless oil. According to GC the product is 89.4% pure.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05260051uspto-grants-1993_11