Reaction #487492

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
   OtherTo a 1000-ml three-neck flask equipped with a stirrer and a condenser
2. 2
   OtherTo this flask, a solution, prepared
3. 3
   workup.ADDITIONwas added dropwise over 3 hours
4. 4
   workup.ADDITIONAfter the completion of the dropwise addition
5. 5
   Otherto react for an additional one hour
6. 6
   Othera solution prepared
7. 7
   workup.ADDITIONwas added
8. 8
   TemperatureThe temperature of the mixture was raised to 78° C.
9. 9
   Temperaturethe mixture was heated for 4 hours
10. 10
    OtherThe resulting reaction solution
11. 11
    Otherwas subjected to re-precipitation twice with an excess amount of hexane
12. 12
    Otherthe precipitated resin was dried

Procedure

To a 1000-ml three-neck flask equipped with a stirrer and a condenser, 88 g of methyl ethyl ketone was added, and heated to 72° C. under a nitrogen atmosphere. To this flask, a solution, prepared 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 dropwise over 3 hours. After the completion of the dropwise addition, the content in the flask was allowed to react for an additional one hour, and then a solution prepared by dissolving 0.42 g of dimethyl-2,2′-azobisisobutyrate in 2 g of methyl ethyl ketone was added thereto. The temperature of the mixture was raised to 78° C., and the mixture was heated for 4 hours. The resulting reaction solution was subjected to re-precipitation twice with an excess amount of hexane, and the precipitated resin was dried. 96.5 g of a phenoxyethyl methacrylate/methyl methacrylate/methacrylic acid copolymer (resin dispersant P-1, copolymerization ratio by mass %=50/37/13) was thus obtained.

Source