반응 #1069770

반응 방정식

acetone

cis-1,2-cyclohexanedicarboxylic anhydride

2-hydroxyethyl methacrylate

→

2-[2-(methacryloyloxy)ethoxy-carbonyl]cyclohexanecarboxylic acid

용매

water

반응 조건

후처리

1. 1
   온도This mixture was heated
2. 2
   온도with refluxing for 5 hours
3. 3
   workup.DISTILLATIONthe acetone was distilled off under reduced pressure
4. 4
   workup.ADDITIONThereafter, 1N hydrochloric acid (500 mL) and ethyl acetate (2,000 mL) were added to the residue
5. 5
   추출to extract it
6. 6
   세척The resulting organic phase was washed twice with saturated aqueous sodium chloride solution (500 mL), and anhydrous magnesium sulfate (100 g)
7. 7
   workup.ADDITIONwas then added
8. 8
   기타Subsequently, the magnesium sulfate was removed by filtration
9. 9
   workup.DISTILLATIONthe ethyl acetate was distilled off under reduced pressure
10. 10
    기타to obtain a white solid
11. 11
    여과the particles were taken out by filtration
12. 12
    기타dried

실험 절차

To acetone (1,000 mL) were added cis-1,2-cyclohexanedicarboxylic anhydride (308.3 g), 2-hydroxyethyl methacrylate (273.3 g), and 4-dimethylaminopyridine (4.9 g). This mixture was heated with refluxing for 5 hours, and the acetone was distilled off under reduced pressure. Thereafter, 1N hydrochloric acid (500 mL) and ethyl acetate (2,000 mL) were added to the residue to extract it. The resulting organic phase was washed twice with saturated aqueous sodium chloride solution (500 mL), and anhydrous magnesium sulfate (100 g) was then added thereto. This mixture was allowed to stand for 1 hour to dehydrate the organic phase. Subsequently, the magnesium sulfate was removed by filtration and the ethyl acetate was distilled off under reduced pressure to obtain a white solid. The solid was pulverized and then added to water (2,000 mL). After this mixture was stirred for 2 hours, the particles were taken out by filtration and dried. As a result, 2-[2-(methacryloyloxy)ethoxy-carbonyl]cyclohexanecarboxylic acid was obtained as a white solid (518.9 g).

출처