HRID2093261

反应详情

EQUATION

反应方程式

HRID 2093261 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

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.

WORKUP

后处理

  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