Reaction #487490

Reaction equation

phenoxyethyl methacrylate

methacrylic acid

methyl methacrylate

→

phenoxyethyl methacrylate methyl methacrylate methacrylic acid

Yield 162.8%

Solvents

methyl ethyl ketone

methyl ethyl ketone

methyl ethyl ketone

Conditions

Workup

1. 1
   Otherequipped with a stirrer and a condenser tube
2. 2
   OtherThen, a solution obtained
3. 3
   workup.ADDITIONwas added
4. 4
   workup.ADDITIONAfter the addition
5. 5
   Otherto react for one hour
6. 6
   Othera solution obtained
7. 7
   workup.ADDITIONwas added
8. 8
   Otherwas elevated to 78° C.
9. 9
   Temperaturethe mixture was heated for 4 hours
10. 10
    OtherThe obtained reaction liquid
11. 11
    Otherwas reprecipitated twice with an excess of hexane
12. 12
    OtherThe separated resin was dried

Procedure

88 g of methyl ethyl ketone was placed in a 1000 mL three-necked flask equipped with a stirrer and a condenser tube, and was heated to 72° C. under a nitrogen atmosphere. Then, a solution obtained by dissolving 0.85 g of dimethyl 2,2′-azobisisobutyrate, 50 g of phenoxyethyl methacrylate, 13 g of methacrylic acid, and 37 g of methyl methacrylate in 50 g of methyl ethyl ketone was added thereto dropwise over 3 hours. After the addition was completed, the mixture was further allowed to react for one hour, and then a solution obtained by dissolving 0.42 g of dimethyl 2,2′-azobisisobutyrate in 2 g of methyl ethyl ketone was added thereto. The temperature of the resulting mixture was elevated to 78° C., and the mixture was heated for 4 hours. The obtained reaction liquid was reprecipitated twice with an excess of hexane. The separated resin was dried, to obtain 96.5 g of a phenoxyethyl methacrylate/methyl methacrylate/methacrylic acid (copolymerization ratio [mass % ratio]=50/37/13) copolymer (polymer dispersant P-1).

Source