Methacrylic Acid → 1-(2-Methylpropoxy)ethyl 2-methylprop-2-enoate

Into a 50-mL eggplant-shaped flask, 8.61 g (100 mmol) of methacrylic acid and 20.0 g (200 mmol) of isobutyl vinyl ether were placed. A fluorine resin-coated stirring piece was dropped into the flask. The mixed solution inside the flask was heated for 6 hours by immersing the flask in an oil bath whose temperature was controlled to 60° C. while stirring the mixed solution by the stirring piece with the use of a magnetic stirrer. After the heating, the whole of the mixed solution was mixed with 20 ml of aqueous sodium hydrogencarbonate solution (concentration: 5 wt %). The resulting mixed solution was left still and separated into an organic phase and an aqueous phase. The organic phase was extracted, dried with sodium sulfate to remove therefrom moisture content, and then, filtrated. The thus-obtained filtrate was concentrated under the conditions of a temperature of 40° C. and a pressure of 30 hPa by a rotary evaporator. By this, 12.32 g of 1-(2-methylpropoxy)ethyl methacrylate of the following formula was obtained in the form of a pale yellow liquid as a protected carboxyl-containing monomer for providing a repeating unit B2 in a polymer.

1. temperatureThe mixed solution inside the flask was heated for 6 hours
2. customwas controlled to 60° C.
3. additionThe resulting mixed solution
4. waitwas left still
5. customseparated into an organic phase
6. extractionThe organic phase was extracted
7. dry with materialdried with sodium sulfate
8. customto remove
9. filtrationmoisture content, and then, filtrated
10. concentrationThe thus-obtained filtrate was concentrated under the conditions of a temperature of 40° C.
11. customa pressure of 30 hPa by a rotary evaporator

ORD record

ord-d35e1a8f6fdb466f9c51b0c9ea4ce141

Source dataset

uspto-grants-2016_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09310682B2