HRID396732

反应详情

EQUATION

反应方程式

HRID 396732 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

23.8 g (0.06 mol) of 2-(2,4-dihydroxyphenyl)-4,6-bis-(2,4-dimethylphenyl)-1,3,5-triazine (prepared as described in U.S. Pat. No. 3,244,708 Example 16) are suspended in 300 ml of xylene. 12.1 g (0.09 mol) of 97% butyl glycidyl ether and 0.75 g (0.006 mol) of dimethylbenzylamine are added to this suspension, and the mixture is heated to reflux temperature. After a reaction time of 5 hours the clear, brownish solution is cooled and clarified by filtration through 100 g of silica gel. The yellow solution is evaporated and the residue is recrystallized from hexane/toluene. This gives 27.3 g of pale yellow crystals of 2-[2-hydroxy-4(3-butoxy-2-hydroxypropyloxy)-phenyl]-4,6-bis(2,4-dimethylphenyl)-1,3,5-triazin (=86% yield). Melting point: 80-83° C. (Compound 1).

WORKUP

后处理

  1. temperaturethe mixture is heated
  2. temperatureto reflux temperature
  3. temperatureAfter a reaction time of 5 hours the clear, brownish solution is cooled
  4. filtrationclarified by filtration through 100 g of silica gel
  5. customThe yellow solution is evaporated
  6. customthe residue is recrystallized from hexane/toluene