反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- -20 °C
PROCEDURE
实验过程
A 4-necked 5-L flask, equipped with a mechanical stirrer, a thermometer, and an additional funnel, is charged with methyl isobutyl ketone (1500 g), 1,1-dichloro-2,2-bis(4-hydroxyphenyl)ethene (320 g), and cyanogen bromide (270 g). The resulting solution is cooled to −20° C. with a dry ice/acetone bath. To the stirring solution, triethylamine (240 g) in the additional funnel is added dropwise. The reaction temperature is maintained below −20° C. After the addition, the resulting mixture is allowed to warm up to 0° C. and quenched with dilute HCl aqueous solution. The organic layer is washed further with water a few times and concentrated under vacuum to afford 370 g of amber liquid, which solidifies as light tan color solids.
WORKUP
后处理
- customA 4-necked 5-L flask, equipped with a mechanical stirrer
- temperatureThe reaction temperature is maintained below −20° C
- additionAfter the addition
- temperatureto warm up to 0° C.
- customquenched with dilute HCl aqueous solution
- washThe organic layer is washed further with water a few times
- concentrationconcentrated under vacuum