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3-Hydroxybutyric Acid → Dodecyl 3-Hydroxybutyrate

HRID 2380182
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HRID 2380182 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>>[OH:1][CH:2]([CH3:7])[CH2:3][C:4]([O:6][CH2:19][CH2:18][CH2:17][CH2:16][CH2:15][CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][CH3:8])=[O:5]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 4413-Hydroxybutyric AcidHCID 1118Sulfuric AcidHCID 81931-Dodecanol

생성물 1

HCID 18955122Dodecyl 3-Hydroxybutyrate수율 117.65%

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온도
120 °C

실험 절차

A 500 mL one neck round bottom flask equipped with a Dean Stark trap, condenser, and a nitrogen inlet/outlet was charged with 72.0 g (69 mmole) of 3-hydroxybutyric acid, 268.5 g (1.45 mole) of dodecyl alcohol, and 0.36 g of sulfuric acid. The mixture was heated to 120° C. for 48 hours and water was collected as the reaction proceeded. The acid was neutralized by washing three times with 100 mL saturated NaHCO3 solution. The organic layer was collected and dried over MgSO4 and concentrated. Excess dodecanol was removed by high vacuum distillation to yield 117.65% (60% yield) of clear oil (91% pure by GC).

후처리

  1. customwater was collected as the reaction
  2. washby washing three times with 100 mL saturated NaHCO3 solution
  3. customThe organic layer was collected
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated
  6. customExcess dodecanol was removed by high vacuum distillation

출처 및 근거

ORD 기록
ord-42787cf725b047e0bc59a10aa1987dc9
출처 데이터셋
uspto-grants-1994_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05366665

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