反応式
[C:1]1([C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[OH:4])[OH:2].C/C(/O)=C/C(C)=O.C/C(/O)=C/C(C)=O.C/C(/O)=C/C(C)=O.[V:30]>C1(C)C(C)=CC=CC=1>[C:1]1([C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[O-:4])[O-:2].[V+5:30].[C:1]1([C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[O-:4])[O-:2].[C:1]1([C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[O-:4])[O-:2].[C:1]1([C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[O-:4])[O-:2].[C:1]1([C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[O-:4])[O-:2].[V+5:30]参加物
反応条件
- 温度
- 100 °C
実験手順
A solution of catechol (3.30 g, 30 mmol) and xylene (45 ml) was dehydrated by distilling 5 mL of the solution. Thereafter, 6.97 g (20 mmol) of vanadium(III) acetylacetonate was added to the solution while stirring. The mixed solution was refluxed for 1 hour, and then, while the distillation temperature was 132° 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-vanadium complex) was black in color. The yield amount was 4.26 g (20.0 mmol), and the yield percentage was 100%. Catechol-vanadium complex was dissolved into acetylacetone until saturated, and then filtered to be used as a coating liquid.
後処理
- distillationby distilling 5 mL of the solution
- temperatureThe mixed solution was refluxed for 1 hour
- customwas 132° C.
- distillationhigher, distilled until the amount of the solution
- distillationAfter the distillation, solid content of the product
- customwas isolated by suction
- filtrationfiltering
- filtrationfilter
- customwere completely removed
- dissolutionCatechol-vanadium complex was dissolved into acetylacetone until saturated, and
- filtrationthen filtered
出典と根拠
- ORDレコード
- ord-078a37fa1f284f388bd2cc199bffb787
- 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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