Catechol → HCID 178515958、化合物

HRID 2093261

反応式

HRID 2093261 の反応式
[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

4

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

  1. distillationby distilling 5 mL of the solution
  2. temperatureThe mixed solution was refluxed for 1 hour
  3. customwas 132° 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
  10. dissolutionCatechol-vanadium complex was dissolved into acetylacetone until saturated, and
  11. 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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