反应 #2775

反应方程式

hydroquinone

methacryloyl chloride

→

hydroquinone monomethacrylate

溶剂

pyridine

acetone

反应条件

后处理

1. 1
   温度maintained at 0° to 5° C
2. 2
   workup.STIRRINGAfter stirring for one more hour at room temperature
3. 3
   其他the acetone was evaporated
4. 4
   workup.ADDITIONWater was then added
5. 5
   萃取with ether extraction
6. 6
   洗涤After washing this ether layer with a 5% aqueous solution of sodium hydrogencarbonate
7. 7
   洗涤the solution was then washed with water
8. 8
   干燥dried (anhydrous sodium carbonate)
9. 9
   其他The ether was then evaporated out, with a white solid being
10. 10
    其他obtained
11. 11
    其他This was recrystallized from water

实验过程

350 g of hydroquinone was dissolved in 2.5 kg of acetone and 500 ml of pyridine. After cooling to 0° C., 313.5 g of methacryloyl chloride was added dropwise, with the reaction temperature maintained at 0° to 5° C. Stirring was then carried out for 3 hours at the same temperature. After stirring for one more hour at room temperature, the acetone was evaporated. Water was then added, and hydrochloric acid was used to adjust the solution to an acidic pH (pH 4), with ether extraction then performed. After washing this ether layer with a 5% aqueous solution of sodium hydrogencarbonate, the solution was then washed with water and dried (anhydrous sodium carbonate). The ether was then evaporated out, with a white solid being obtained. This was recrystallized from water, to obtain 420 g of colorless, needle crystals of hydroquinone monomethacrylate having a melting point of 120.5° to 121.5° C.

来源