HRID1590950

反应详情

EQUATION

反应方程式

HRID 1590950 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
118 °C

PROCEDURE

实验过程

A mixture of 75 g (156 mmol) of bis(2,2,6,6-tetramethylpiperidin-4-yl)sebacate, 1.3 g of molybdenum trioxide, and 475 ml of cyclooctane is heated to 118° C. To this mixture is added 130 g (1.01 mol) of 70% aq. t-butyl hydroperoxide during a 5 hour period. The reaction mixture is maintained at reflux during the addition, and water is collected in a Dean-Stark trap. The red reaction mixture is heated for 7 hours after the addition to discharge the red color. Solids are removed by filtration, and the filtrate is evaporated to give a yellow oil. Purification (Waters Prep. 500 A HPLC, 20:1 hexane: ethyl acetate) affords 78.7 g (68%) of the title compound, a colorless syrup.

WORKUP

后处理

  1. temperatureThe reaction mixture is maintained
  2. customis collected in a Dean-Stark trap
  3. customThe red reaction mixture
  4. temperatureis heated for 7 hours
  5. additionafter the addition
  6. customSolids are removed by filtration
  7. customthe filtrate is evaporated
  8. customto give a yellow oil
  9. customPurification (Waters Prep