Glycerol → HCID 86708448, 화합물

HRID 1404731노트

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HRID 1404731 반응식
[OH:1][CH2:2][CH:3]([CH2:5][OH:6])[OH:4].[C:7]([O:14][CH3:15])(=O)[CH2:8][CH2:9][CH2:10][CH2:11][CH3:12]>[Pd]>[CH2:7]([O:1][CH2:2][CH:3]([CH2:5][OH:6])[OH:4])[CH2:8][CH2:9][CH2:10][CH2:11][CH3:12].[CH3:2][CH2:15][O:14][CH2:7][CH3:8]

참가 물질

4

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온도
140 °C

실험 절차

A stirred autoclave was charged, at room temperature, with 55.2 g (600 mmol) of glycerol, 3.9 g (30 mmol) of methyl caproate, 0.39 g (10 wt %) of camphosulfonic acid and 0.3 g (0.5 mol %) of Pd/C at 5%. The autoclave was then pressurized at 10 bar of dihydrogen gas H2, and then it was heated at 140° C. for 24 h, stirring vigorously. After 24 h of reaction, the reaction mixture was brought back to room temperature. The catalyst was filtered on a MILLIPORE® filter (a membrane filter) (0.45 μm) and was rinsed with absolute ethanol. The solvents were evaporated and the organic products were extracted from the glycerol phase by extraction with CH2Cl2 (3×50 ml). The organic phase was washed with water (2×30 ml) and the CH2Cl2 was then evaporated at reduced pressure. The crude reaction product was analyzed by GC/MS. 1-O-hexyl-glycerol ether was obtained at 22% GC yield.

후처리

  1. customAfter 24 h of reaction
  2. customwas brought back to room temperature
  3. filtrationThe catalyst was filtered on a MILLIPORE®
  4. filtrationfilter (a membrane
  5. filtrationfilter) (0.45 μm)
  6. washwas rinsed with absolute ethanol
  7. customThe solvents were evaporated
  8. extractionthe organic products were extracted from the glycerol phase by extraction with CH2Cl2 (3×50 ml)
  9. washThe organic phase was washed with water (2×30 ml)
  10. customthe CH2Cl2 was then evaporated at reduced pressure
  11. customThe crude reaction product

출처 및 근거

ORD 기록
ord-e3c2b286e0654bc6acfe2d1b9b423ee6
출처 데이터셋
uspto-grants-2014_12
특허 번호
US08912365B2

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