HRID1490390

反应详情

EQUATION

反应方程式

HRID 1490390 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

To a 350 mL sulfonation flask equipped with a mechanical stirrer, condenser and a nitrogen atmosphere are charged 29.6 g (100 mmol) of 2-chloro-4,6-bis(4-methylphenyl)-s-triazine, and 100 mL of xylene (mixture of isomers). To the beige suspension are added 11.3 g (85 mmol) of aluminum chloride in one portion. The mixture is warmed to ca. 90° C. for 75 minutes. 21.4 g (110 mmol) of 4-hexylresorcinol are then added in five portions over 45 minutes to the now homogeneous solution. The reaction mixture is heated at 90° C. for 18 hours. After cooling to room temperature, the contents of the flask are poured into 120 mL of 6% aqueous hydrochloric acid. The precipitate formed is removed by filtration, washed to pH 7 with water, rinsed with methanol and dried at 70° C. under vacuum. The title compound is obtained as a crude orange product (43.1 g) and melts at 228°-231° C. It can be used without further purification.

WORKUP

后处理

  1. customTo a 350 mL sulfonation flask equipped with a mechanical stirrer, condenser
  2. temperatureThe reaction mixture is heated at 90° C. for 18 hours
  3. temperatureAfter cooling to room temperature
  4. customThe precipitate formed
  5. customis removed by filtration
  6. washwashed to pH 7 with water
  7. washrinsed with methanol
  8. customdried at 70° C. under vacuum