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Catechol → HCID 131730579、化合物

HRID 2093263
ノート
印刷プレビュー

反応式

HRID 2093263 の反応式
[C:1]1([C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[OH:4])[OH:2].[O-]CC.[Ta+5:12].[O-]CC.[O-]CC.[O-]CC.[O-]CC>C1(C)C=CC=CC=1>[C:1]1([C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[O-:4])[O-:2].[Ta+5:12].[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].[Ta+5:12]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 289CatecholHCID 160806ethanol, tantalum(5+) salt

生成物 1

HCID 131730579HCID 131730579、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
100 °C

実験手順

A solution of catechol (5.51 g, 50.0 mmol) and toluene (50 ml) was dehydrated by distilling 10 mL of the solution. Thereafter, 8.13 g (20.0 mmol) of tantalum(V) ethoxide was added to the solution while stirring. The mixed solution was refluxed for 1 hour, and then, while the distillation temperature was 110° C. or higher, distilled until the amount of the solution became half. After the distillation, volatile components of the residual mixed solution were vaporized under reduced pressure by a rotary evaporator. The residual solid content was further heated to 100° C. under vacuum using a vacuum dryer so that the remaining volatile components were completely removed. The solid content (catechol-tantalum complex) was yellow in color. The yield amount was 9.02 g (20.0 mmol), and the yield percentage was 100%. 4.51 g of catechol-tantalum complex was dissolved into 100 mL of 1:4 acetylacetone/toluene to produce a coating liquid.

後処理

  1. distillationby distilling 10 mL of the solution
  2. temperatureThe mixed solution was refluxed for 1 hour
  3. customwas 110° C.
  4. distillationhigher, distilled until the amount of the solution
  5. distillationAfter the distillation, volatile components of the residual mixed solution
  6. customwere vaporized under reduced pressure by a rotary evaporator
  7. customwere completely removed
  8. dissolution4.51 g of catechol-tantalum complex was dissolved into 100 mL of 1:4 acetylacetone/toluene
  9. customto produce a coating liquid

出典と根拠

ORDレコード
ord-c7c14900ec68494d8fd39675a1ebd507
出典データセット
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08445118B2

反応ノート

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