HRID265822

反应详情

EQUATION

反应方程式

HRID 265822 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
175 °C

PROCEDURE

实验过程

To a 1 L three-necked, round-bottomed flask equipped with a magnetic stirrer, condenser, dropping funnel, thermometer, and a nitrogen atmosphere are charged 15.0 g (37.8 mmol) of 2-(2,4-dihydroxyphenyl)-4,6-bis-(2,4-dimethylphenyl)-s-triazine and 390 mg of aluminum isopropoxide. The mixture is heated to 175° C. and 4.47 g (37.9 mmol) of α-methylstyrene are added dropwise at a rate of one drop every two seconds. A total of six equivalents of or-methyl styrene are added in this fashion over a 4.5 hour period. After cooling to room temperature, the mixture is diluted with ethyl acetate, washed twice with water and once with brine, and is dried over anhydrous magnesium sulfate. Following filtration, the solvent is removed under reduced pressure to yield a yellow solid. The crude product is purified with medium pressure chromatography with 12% ethyl acetate/heptane to afford 13.2 g of the title compound as a yellow solid; mp 168°-170° C.

WORKUP

后处理

  1. customTo a 1 L three-necked, round-bottomed flask equipped with a magnetic stirrer, condenser
  2. temperatureAfter cooling to room temperature
  3. washwashed twice with water and once with brine
  4. dry with materialis dried over anhydrous magnesium sulfate
  5. filtrationfiltration
  6. customthe solvent is removed under reduced pressure
  7. customto yield a yellow solid
  8. customThe crude product is purified with medium pressure chromatography with 12% ethyl acetate/heptane