Acetic Acid → Methoxy(ethoxy)acetate acetate alumoxane

HRID 586108

反応式

HRID 586108 の反応式
[C:1]([OH:4])(=[O:3])[CH3:2].[CH3:5][O:6][CH:7]([O:11][CH2:12][CH3:13])[C:8]([OH:10])=[O:9].C(OCC)C.[AlH:19]1[CH2:24][CH2:23][CH2:22][CH2:21][O:20]1>O.C(O)C>[CH3:5][O:6][CH:7]([O:11][CH2:12][CH3:13])[C:8]([O-:10])=[O:9].[C:1]([O-:4])(=[O:3])[CH3:2].[AlH:19]1[CH2:24][CH2:23][CH2:22][CH2:21][O:20]1

参加物

7

反応物 4

HCID 176Acetic AcidHCID 3283Diethyl EtherHCID 22259842HCID 22259842、化合物HCID 131716739Oxaluminane

生成物 1

HCID 131725076Methoxy(ethoxy)acetate acetate alumoxane

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

Acetic acid (19.0 mL) and methoxy(ethoxy) acetic acid (152.0 mL) was dissolved in 500 mL of water and Vista Captal B boehmite (20 g) was slowly added and refluxed for 72 hours. The white solution was filtered and the filtrate was dissolved under reduced pressure to yield a brown gel. The gel was dissolved in ethanol (100 mL) and the white powder product was obtained by the addition of diethyl ether. Yield: 8.9 g. The TGA of the product showed 32.5% ceramic yield (weight loss of 67.5%). 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.

後処理

  1. temperaturerefluxed for 72 hours
  2. filtrationThe white solution was filtered
  3. dissolutionthe filtrate was dissolved under reduced pressure
  4. customto yield a brown gel
  5. customceramic yield (weight loss of 67.5%)
  6. customfollowed by a temperature ramp up to 1000° C. at the rate of 5° C.min−1
  7. waitsoaked for 2 h.

出典と根拠

ORDレコード
ord-b2476ee4a8b2452e9748bc179686f91e
出典データセット
uspto-grants-2005_08
特許番号
US06936306B1

関連ノート

読み込み中…