HRID1590950
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe reaction mixture is maintained
- customis collected in a Dean-Stark trap
- customThe red reaction mixture
- temperatureis heated for 7 hours
- additionafter the addition
- customSolids are removed by filtration
- customthe filtrate is evaporated
- customto give a yellow oil
- customPurification (Waters Prep