Methoxy(ethoxyethoxy)acetic acid → Methoxy(ethoxyethoxy)acetate alumoxane

HRID 586105

Reaktionsgleichung

Reaktionsgleichung von HRID 586105
[CH3:1][O:2][CH:3]([O:7][CH2:8][CH2:9][O:10][CH2:11][CH3:12])[C:4]([OH:6])=[O:5].COC(OCC)C([O-])=O.[AlH:22]1[CH2:27][CH2:26][CH2:25][CH2:24][O:23]1.[AlH]1CCCCO1>O>[CH3:1][O:2][CH:3]([O:7][CH2:8][CH2:9][O:10][CH2:11][CH3:12])[C:4]([O-:6])=[O:5].[AlH:22]1[CH2:27][CH2:26][CH2:25][CH2:24][O:23]1

Komponenten

5

Edukt 3

HCID 11376371Methoxy(ethoxyethoxy)acetic acidHCID 131716739OxaluminaneHCID 131725073Methoxy(ethoxy)acetate alumoxane

Produkt 1

HCID 131725072Methoxy(ethoxyethoxy)acetate alumoxane

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

Methoxy(ethoxyethoxy)acetic acid (60 mL) was dissolved in 300 mL of water and Vista Captal B boehmite (12 g) was slowly added and allowed to reflux for 96 hours. The clear/yellow solution was filtered and the filtrate was evaporated under reduced pressure to a yellow gel. The gel was dissolved in ethanol and the white/yellow powder product was obtained upon addition of diethyl ether. Yield: 13.6 g. The TGA of the methoxy(ethoxy)acetate-alumoxane showed 22.3% ceramic yield (weight loss of 77.7% ). 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.

Aufarbeitung

  1. temperatureto reflux for 96 hours
  2. filtrationThe clear/yellow solution was filtered
  3. customthe filtrate was evaporated under reduced pressure to a yellow gel
  4. dissolutionThe gel was dissolved in ethanol
  5. customthe white/yellow powder product was obtained upon addition of diethyl ether
  6. customceramic yield (weight loss of 77.7% )
  7. customfollowed by a temperature ramp up to 1000° C. at the rate of 5° C.min−1
  8. waitsoaked for 2 h.

Quellen und Nachweise

ORD-Eintrag
ord-ff3c978bd0af43c39f6559838a6a6f94
Quelldatensatz
uspto-grants-2005_08
Patentnummer
US06936306B1

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