3-Hydroxybutyric Acid → Decyl 3-hydroxybutanoate

HRID 256796노트

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HRID 256796 반응식
[OH:1][CH:2]([CH3:7])[CH2:3][C:4]([OH:6])=[O:5].[CH2:8](O)[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17]>S(=O)(=O)(O)O>[OH:1][CH:2]([CH3:7])[CH2:3][C:4]([O:6][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17])=[O:5]

참가 물질

4

반응물 2

HCID 4413-Hydroxybutyric AcidHCID 81741-Decanol

생성물 1

HCID 18955013Decyl 3-hydroxybutanoate수율 58%

시약·촉매·용매 1

HCID 1118Sulfuric Acid촉매

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온도
140 °C

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.

후처리

  1. customwater was collected as the reaction
  2. washby washing three times with 50 ml saturated sodium bicarbonate solution
  3. customThe organic layer was collected
  4. dry with materialdried over magnesium sulfate
  5. customExcess decyl alcohol was removed by high vacuum distillation

출처 및 근거

ORD 기록
ord-455d0015f18a471f8d6cd93cf4c68d19
출처 데이터셋
uspto-grants-1993_11
특허 번호
US05260051

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