反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionwas added over 5 mins
- washThe container of slurry was washed two times with 2×50 ml of toluene
- temperatureThe reaction mixture was heated (the reactor
- temperaturewas heated with a 250° C. hot oil
- washThe dark brown mixture was washed with 5% H2SO4 and water
- customThe organic solution was separated
- dry with materialdried over MgSO4
- customRemoval of the solvent
- waitleft dark color oil as crude product
- customThe purification
- distillationwas achieved through vacuums distillation and chromatography