2-Chloroethyl vinyl ether → Vinyloxyethyl methacrylate

온도

80 °C

40 g of sodium methacrylate was suspended in 300 g of dimethylsulfoxide (DMSO) in a 2 L flask equipped with a mechanical stirrer, cold water condenser and heating mantle. 0.35 g of 4-methoxyphenol was added. The mixture was heated to 80° C. with stirring under a nitrogen blanket. During heating, 36 g of 2-chloroethyl vinyl ether was added over 30 minutes. The reaction was then maintained at 80° C. for 20 hr. After the reaction solution was cooled to room temperature, 0.45 g of sodium hydroxide dissolved in 300 ml of water was added and the mixture was stirred for 20 minutes. About 500 g of chloroform was then added and the resulting mixture was stirred for 30 minutes. The mixture was then transferred into a separatory funnel. The bottom layer was separated and discarded. The chloroform layer was washed thoroughly with deionized (Dl) water and dried with sodium sulfate. The filtrate was then subjected to rotary evaporation at room temperature to remove most of the volatile materials. The lightly colored liquid was consistent with 2-vinyloxyethyl methacrylate (VEMA) by proton NMR: (in CDCl3): 1.98 ppm (3H CH3), 3.8 ppm (2H C(O)CH2CH2-O), 4.3 ppm (2 H C(O)CH2CH2-O), 4.0 ppm and 4.2 ppm (2H OCHCH2), 5.5 ppm and 6.2 ppm (2H CH2=C(CH3)), 6.5 ppm (1H OCHCH2).

1. customequipped with a mechanical stirrer, cold water condenser
2. temperatureheating mantle
3. temperatureDuring heating
4. temperatureThe reaction was then maintained at 80° C. for 20 hr
5. temperatureAfter the reaction solution was cooled to room temperature
6. additionwas added
7. stirringthe mixture was stirred for 20 minutes
8. stirringthe resulting mixture was stirred for 30 minutes
9. customThe mixture was then transferred into a separatory funnel
10. customThe bottom layer was separated
11. washThe chloroform layer was washed thoroughly with deionized (Dl) water
12. dry with materialdried with sodium sulfate
13. customThe filtrate was then subjected to rotary evaporation at room temperature
14. customto remove most of the volatile materials

ORD 기록

ord-34d8f2c329284967a9f1de1695f48fe4

출처 데이터셋

uspto-grants-2015_07

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US09093263B2