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3-Hydroxybutyric Acid → Dodecyl 3-Hydroxybutyrate

HRID 256799
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HRID 256799 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][CH2:17][CH2:18][CH3:19]>S(=O)(=O)(O)O>[CH2:19]([O:5][C:4](=[O:6])[CH2:3][CH:2]([OH:1])[CH3:7])[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][CH3:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 4413-Hydroxybutyric AcidHCID 81931-Dodecanol

생성물 1

HCID 18955122Dodecyl 3-Hydroxybutyrate수율 62.6%

시약·촉매·용매 1

HCID 1118Sulfuric Acid촉매

실험 절차

A 500 ml one neck round bottom flask equipped with a Dean Stark trap, condenser and nitrogen inlet/outlet was charged with 72.0 g (0.69 moles) 3- hydroxybutyric acid, 268.5 g (1.45 moles) dodecyl alcohol, and 0.36 g sulfuric acid (based on 0.5 g/mole 3-hydroxybutyric acid). The mixture was heated to 115 degrees for 48 hours and water was collected as the reaction proceeded. The acid was neutralized by washing three times with 100 ml saturated sodium bicarbonate solution. The organic layer was collected and dried over magnesium sulfate. Excess dodecyl alcohol was removed by high vacuum distillation to yield 117.65 g (60% yield) of clear oil (91% pure by GC).

후처리

  1. temperatureThe mixture was heated to 115 degrees for 48 hours
  2. customwater was collected as the reaction
  3. washby washing three times with 100 ml saturated sodium bicarbonate solution
  4. customThe organic layer was collected
  5. dry with materialdried over magnesium sulfate
  6. customExcess dodecyl alcohol was removed by high vacuum distillation

출처 및 근거

ORD 기록
ord-a47b2d80e9cc48ca9fbd823d760c630e
출처 데이터셋
uspto-grants-1993_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05260051

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