HRID2093262

反应详情

EQUATION

反应方程式

HRID 2093262 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 (8.64 g, 78.5 mmol) and toluene (70 ml) was dehydrated by distilling 10 mL of the solution. Thereafter, 10.0 g (31.4 mmol) of niobium(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-niobium complex) was brown in color. The yield amount was 11.4 g (31.4 mmol), and the yield percentage was 100%. 3.63 g of catechol-niobium complex was dissolved into 100 mL of 1:4 acetylacetone/toluene to produce a coating liquid.

WORKUP

后处理

  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. dissolution3.63 g of catechol-niobium complex was dissolved into 100 mL of 1:4 acetylacetone/toluene
  9. customto produce a coating liquid