Dimethyl Sulfoxide → Acrylic acid hydroxyethyl methacrylate

HRID 931872노트

반응식

HRID 931872 반응식
[C:1]([O:6][CH2:7][CH2:8][OH:9])(=[O:5])[C:2]([CH3:4])=[CH2:3].[C:10]([OH:14])(=[O:13])[CH:11]=[CH2:12].CS(C)=O.N(C(C1NCCN=1)(C)C)=NC(C1NCCN=1)(C)C>C(O)C.O>[C:1]([O:6][CH2:7][CH2:8][OH:9])(=[O:5])[C:2]([CH3:4])=[CH2:3].[C:10]([OH:14])(=[O:13])[CH:11]=[CH2:12]

참가 물질

7

반응물 4

HCID 679Dimethyl SulfoxideHCID 6581Acrylic AcidHCID 133602-Hydroxyethyl MethacrylateHCID 887152,2'-Azobis(2-(2-imidazolin-2-yl)propane)

생성물 1

HCID 10330472Acrylic acid hydroxyethyl methacrylate

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

In a 200 mL three-necked flask, 2-hydroxyethyl methacrylate (HEMA, 11.4 g, 0.10 mol), acrylic acid (AA, 7.21 g, 0.10 mol), dimethyl sulfoxide (74.5 g) and a polymerization initiator VA-061 (Wako Pure Chemical Industries, Ltd., 0.016 g, 0.062 mmol) were charged, and then equipped with a three-way stop-cock, a reflux condenser tube, a thermometer and a mechanical stirrer. The concentration of the monomer was 20% by weight. After degassing inside the three-necked flask using a vacuum pump and repeating replacement by argon three times, stirring was carried out at 60° C. for 0.5 hours, followed by temperature rise to 70° C. and further stirring for 6.5 hours. After completion of the polymerization, the polymerization reaction solution was cooled to room temperature, and then the mixed solution was poured into water (1,000 mL)/ethanol (10 mL) and left to stand overnight. On the next day, the supernatant was discarded and the obtained solid component was further washed twice with 700 mL of water. The solid component was dried overnight by a vacuum drying oven at 60° C. Liquid nitrogen was charged and the solid component was crushed by a spatula, and then dried by a vacuum drying oven at 60° C. for 3 hours. The thus obtained copolymer had a molecular weight of Mn: 79 kD, Mw: 226 kD (Mw/Mn=2.9).

후처리

  1. customequipped with a three-way
  2. customAfter degassing inside the three-necked flask
  3. customfollowed by temperature rise to 70° C.
  4. stirringfurther stirring for 6.5 hours
  5. customAfter completion of the polymerization
  6. customthe polymerization reaction solution
  7. waitleft
  8. waitto stand overnight
  9. washthe obtained solid component was further washed twice with 700 mL of water
  10. customThe solid component was dried overnight by a vacuum
  11. customdrying oven at 60° C
  12. additionLiquid nitrogen was charged
  13. customthe solid component was crushed by a spatula
  14. customdried by a vacuum
  15. customdrying oven at 60° C. for 3 hours

출처 및 근거

ORD 기록
ord-2b54e1faa88d4849a74cd0f04fbb6b9e
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09297930B2

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