HRID376489

反应详情

EQUATION

反应方程式

HRID 376489 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
32.5 °C

PROCEDURE

实验过程

8-Quinolinol (1.45 g, 0.010 mol) is added to a three-neck flask with heptane (30 mL), and the mixture is stirred under nitrogen at 25 to 40° C. for 0.5 h. It becomes a pale yellow suspension. Titanium tetrachloride (10 mL of 1.0 M solution in heptane, 0.010 mol) is added dropwise to the suspension. After stirring at 25° C. for 2 h, solvents are removed under vacuum. The product is washed with heptane (30 mL), and the washings are decanted. The residue is dried under vacuum for 1 h, and is then recrystallized from a mixture of hydrocarbon solvents to give purple crystals of 8-quinolinoxytitanium trichloride (2.85 g, 95%).

WORKUP

后处理

  1. stirringAfter stirring at 25° C. for 2 h
  2. customsolvents are removed under vacuum
  3. washThe product is washed with heptane (30 mL)
  4. customthe washings are decanted
  5. customThe residue is dried under vacuum for 1 h
  6. customis then recrystallized from a mixture of hydrocarbon solvents