2-Methyl-2-butanol → N-(2-hydroxyethyl)acrylamide N,N-dimethylacrylamide

HRID 931868

반응식

HRID 931868 반응식
[OH:1][CH2:2][CH2:3][NH:4][C:5](=[O:8])[CH:6]=[CH2:7].[CH3:9][N:10]([CH3:15])[C:11](=[O:14])[CH:12]=[CH2:13].C(O)(CC)(C)C.N(C(C1NCCN=1)(C)C)=NC(C1NCCN=1)(C)C>>[OH:1][CH2:2][CH2:3][NH:4][C:5](=[O:8])[CH:6]=[CH2:7].[CH3:9][N:10]([CH3:15])[C:11](=[O:14])[CH:12]=[CH2:13]

참가 물질

5

반응물 4

HCID 64052-Methyl-2-butanolHCID 17587N,N-DimethylacrylamideHCID 887152,2'-Azobis(2-(2-imidazolin-2-yl)propane)HCID 193628N-(2-Hydroxyethyl)acrylamide (stabilized with MEHQ)

생성물 1

HCID 86674668N-(2-hydroxyethyl)acrylamide N,N-dimethylacrylamide

실험 절차

In a 300 mL three-necked flask, N-(2-hydroxyethyl)acrylamide (15.04 g, 0.100 mol), N,N-dimethylacrylamide (9.96 g, 0.100 mol), t-amyl alcohol (99.80 g), polymerization initiator VA-061 (Wako Pure Chemical Industries, Ltd., 0.0310 g, 0.124 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 70° C. for 1 hour, followed by temperature rise to 75° C. and further stirring for 4 hours. After completion of the polymerization, the polymerization reaction solution was cooled to room temperature and the solvent was distilled off by an evaporator, and then washed once with each of n-hexane/methanol (=200 mL/100 mL, 200 mL/100 mL, 100 mL/40 mL and 100 mL/60 mL). 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: 109 kD, Mw: 660 kD (Mw/Mn=6.1).

후처리

  1. additionwere charged
  2. customequipped with a three-way
  3. customAfter degassing inside the three-necked flask
  4. customfollowed by temperature rise to 75° C.
  5. stirringfurther stirring for 4 hours
  6. customAfter completion of the polymerization
  7. customthe polymerization reaction solution
  8. distillationthe solvent was distilled off by an evaporator
  9. washwashed once with each of n-hexane/methanol (=200 mL/100 mL, 200 mL/100 mL, 100 mL/40 mL and 100 mL/60 mL)
  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-ae23100996944c9cadd4ac212c3d2e7a
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09297930B2

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