HRID987370

反应详情

EQUATION

反应方程式

HRID 987370 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
218 °C

PROCEDURE

实验过程

A pressure reactor was charged with 500 ml of toluene and heated to 218° C. A slurry of a mixture of 2-methoxy-4-nonylphenol (250.4 g, 1.0 mol), paraformaldehyde (94.5 g, 3.15 mol), titanium cresylate (2 ml) and 50 ml of toluene was added over 5 mins. The container of slurry was washed two times with 2×50 ml of toluene. The reaction mixture was heated (the reactor was heated with a 250° C. hot oil circulating through internal coil) and stirred for 25 mins. and discharged from the reactor. The dark brown mixture was washed with 5% H2SO4 and water. The organic solution was separated and dried over MgSO4. Removal of the solvent left dark color oil as crude product. The purification was achieved through vacuums distillation and chromatography.

WORKUP

后处理

  1. additionwas added over 5 mins
  2. washThe container of slurry was washed two times with 2×50 ml of toluene
  3. temperatureThe reaction mixture was heated (the reactor
  4. temperaturewas heated with a 250° C. hot oil
  5. washThe dark brown mixture was washed with 5% H2SO4 and water
  6. customThe organic solution was separated
  7. dry with materialdried over MgSO4
  8. customRemoval of the solvent
  9. waitleft dark color oil as crude product
  10. customThe purification
  11. distillationwas achieved through vacuums distillation and chromatography