Acetic Acid → Methoxy(ethoxyethoxy)acetate acetate alumoxane

HRID 586109

Reaction equation

HRID 586109 reaction equation
[C:1]([OH:4])(=[O:3])[CH3:2].[CH3:5][O:6][CH:7]([O:11][CH2:12][CH2:13][O:14][CH2:15][CH3:16])[C:8]([OH:10])=[O:9].[AlH:17]1[CH2:22][CH2:21][CH2:20][CH2:19][O:18]1>O.C(O)C>[CH3:5][O:6][CH:7]([O:11][CH2:12][CH2:13][O:14][CH2:15][CH3:16])[C:8]([O-:10])=[O:9].[C:1]([O-:4])(=[O:3])[CH3:2].[AlH:17]1[CH2:22][CH2:21][CH2:20][CH2:19][O:18]1

Participants

6

Reactant 3

HCID 176Acetic AcidHCID 11376371Methoxy(ethoxyethoxy)acetic acidHCID 131716739Oxaluminane

Product 1

HCID 131725077Methoxy(ethoxyethoxy)acetate acetate alumoxane

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 962WaterSolvent

Procedure

Acetic acid (28.6 mL) and methoxy(ethoxyethoxy) acetic acid (76.7 mL) was dissolved in 500 mL of water and Vista Captal B boehmite (20 g) was slowly added and the solution was allowed to reflux for 72 hours. The solution was filtered and the filtrate was evaporated under reduced pressure resulting in a white/clear gel. The gel was dissolved in ethanol and the product was collected as a white powder upon the addition of diethyl ether. Yield: 25.4 g. The TGA of the product showed a 28.5% ceramic yield (weight loss of 71.5%). The alumoxane was heated from 25° C. to 200° C. at the rate of 1.5° C.min−1, soaked for 2 h. at 200° C. followed by a temperature ramp up to 1000° C. at the rate of 5° C.min−1, soaked for 2 h.

Workup

  1. temperatureto reflux for 72 hours
  2. filtrationThe solution was filtered
  3. customthe filtrate was evaporated under reduced pressure
  4. customresulting in a white/clear gel
  5. customthe product was collected as a white powder upon the addition of diethyl ether
  6. customceramic yield (weight loss of 71.5%)
  7. customfollowed by a temperature ramp up to 1000° C. at the rate of 5° C.min−1
  8. waitsoaked for 2 h.

Sources & evidence

ORD record
ord-e4183cfa1930456594e412602a19b9e4
Source dataset
uspto-grants-2005_08
Patent number
US06936306B1

Linked notes

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