반응 #2775

반응 방정식

hydroquinone

methacryloyl chloride

→

hydroquinone monomethacrylate

용매

pyridine

acetone

반응 조건

후처리

1. 1
   온도maintained at 0° to 5° C
2. 2
   workup.STIRRINGAfter stirring for one more hour at room temperature
3. 3
   기타the acetone was evaporated
4. 4
   workup.ADDITIONWater was then added
5. 5
   추출with ether extraction
6. 6
   세척After washing this ether layer with a 5% aqueous solution of sodium hydrogencarbonate
7. 7
   세척the solution was then washed with water
8. 8
   건조dried (anhydrous sodium carbonate)
9. 9
   기타The ether was then evaporated out, with a white solid being
10. 10
    기타obtained
11. 11
    기타This was recrystallized from water

실험 절차

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.

출처