Catechol → Zirconium Catecholate

HRID 2093259

反応式

HRID 2093259 の反応式
[C:1]1([C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[OH:4])[OH:2].CC(C)[O-].[Zr+4:13].CC(C)[O-].CC(C)[O-].CC(C)[O-]>C1(C)C=CC=CC=1>[C:1]1([C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[O-:4])[O-:2].[Zr+4:13].[C:1]1([C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[O-:4])[O-:2]

参加物

4

反応条件

温度
100 °C

実験手順

A solution of catechol (2.20 g, 20 mmol) and toluene (25 ml) was dehydrated by distilling 5 mL of the solution. Thereafter, 5.00 g (10.6 mmol) of zirconium(IV) isopropoxide was added to the solution while stirring. The mixed solution was refluxed for 1 hour, and then, while the distillation temperature was 100° C. or higher, distilled until the amount of the solution became half. After the distillation, solid content of the product was isolated by suction filtering using a membrane suction filter. The residual solid content was heated to 100° C. under vacuum using a vacuum dryer so that remaining volatile components were completely removed. The solid content (catechol-zirconium complex) was black in color. The yield amount was 3.07 g (10.0 mmol), and the yield percentage was 100%.

後処理

  1. distillationby distilling 5 mL of the solution
  2. temperatureThe mixed solution was refluxed for 1 hour
  3. customwas 100° C.
  4. distillationhigher, distilled until the amount of the solution
  5. distillationAfter the distillation, solid content of the product
  6. customwas isolated by suction
  7. filtrationfiltering
  8. filtrationfilter
  9. customwere completely removed

出典と根拠

ORDレコード
ord-0cb4ccab636143edbe3653e2050fb660
出典データセット
uspto-grants-2013_05
特許番号
US08445118B2

関連ノート

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