반응 #343978

ord-455d0015f18a471f8d6cd93cf4c68d19

용매

반응 조건

온도
140°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타water was collected as the reaction
  2. 2
    세척by washing three times with 50 ml saturated sodium bicarbonate solution
  3. 3
    기타The organic layer was collected
  4. 4
    건조dried over magnesium sulfate
  5. 5
    기타Excess decyl alcohol was removed by high vacuum distillation

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05260051uspto-grants-1993_11