HRID491278

反应详情

EQUATION

反应方程式

HRID 491278 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Methyl 3,5-di-tert-butyl-4-hydroxyhydrocinnamate (256 g, 0.88 mole) and isooctanol (133 g, 0.91 mole) are added to a laboratory reactor equipped with the necessary auxiliary equipment. The mixture is heated to 85 C under a vacuum of 30 mmHg. After fifteen minutes, the vacuum is released and aluminum isopropoxide (1.77 g, 0.0087 mole, Rhone-Poulenc, Manalox 130) is added. The reaction mass is heated to 130 C while under a vacuum of 75 mmHg. After two hours, the reaction mass is heated to 165 C while under a vacuum of 30 mmHg for one hour. The excess isooctanol is removed by vacuum distillation at 165 C. The title compound (331 g, 97% yield) is obtained as a light yellow oil whose assay is 97% as judged by calibrated gas chromatography.

WORKUP

后处理

  1. customequipped with the necessary auxiliary equipment
  2. temperatureThe mixture is heated to 85 C under a vacuum of 30 mmHg
  3. waitAfter fifteen minutes
  4. temperatureThe reaction mass is heated to 130 C while under a vacuum of 75 mmHg
  5. temperaturethe reaction mass is heated to 165 C while under a vacuum of 30 mmHg for one hour
  6. customThe excess isooctanol is removed by vacuum distillation at 165 C