反应详情

温度

200 °C

Combine 50.6 g. (0.2 mole) of 4,4'-dichlorobenzhydrol with 57.1 g. (0.6 mole) of 2-hydroxy pyridine, with stirring heat to 200° C. and add dropwise 1.0 ml. of concentrated sulfuric acid. Increase the reaction temperature to 240°-250° C. and maintain at that temperature range while collecting water emanating from the reaction. Cool the reaction mixture, add a mixture of ethyl acetate and water with stirring and separate the liquid phases. Dry the organic phase, reduce the volume of ethyl acetate, cool to precipitate the crude product, yield 43 g. Crystallization from ethanol affords the product of this step, m.p. 211°-215° C.

1. additionadd dropwise 1.0 ml
2. temperatureIncrease the reaction temperature to 240°-250° C.
3. temperaturemaintain at that temperature range
4. customwhile collecting water emanating
5. customfrom the reaction
6. temperatureCool the reaction mixture
7. additionadd
8. customseparate the liquid phases
9. customDry the organic phase
10. temperaturecool
11. customto precipitate the crude product, yield 43 g
12. customCrystallization from ethanol
13. customaffords the product of this step, m.p. 211°-215° C.