2-Mercaptoethanol → Acryloylmorpholine N,N-dimethylacrylamide

HRID 931866노트

반응식

HRID 931866 반응식
[C:1]([N:5]1[CH2:10][CH2:9][O:8][CH2:7][CH2:6]1)(=[O:4])[CH:2]=[CH2:3].[CH3:11][N:12]([CH3:17])[C:13](=[O:16])[CH:14]=[CH2:15].C(O)(CC)(C)C.N(C(C1NCCN=1)(C)C)=NC(C1NCCN=1)(C)C.SCCO>>[C:1]([N:5]1[CH2:10][CH2:9][O:8][CH2:7][CH2:6]1)(=[O:4])[CH:2]=[CH2:3].[CH3:11][N:12]([CH3:17])[C:13](=[O:16])[CH:14]=[CH2:15]

참가 물질

6

반응물 5

HCID 15672-MercaptoethanolHCID 64052-Methyl-2-butanolHCID 17587N,N-DimethylacrylamideHCID 887152,2'-Azobis(2-(2-imidazolin-2-yl)propane)HCID 98723Acryloylmorpholine

생성물 1

HCID 131732927Acryloylmorpholine N,N-dimethylacrylamide

실험 절차

In a 300 mL three-necked flask, N-acryloylmorpholine (14.20 g, 0.101 mol), N,N-dimethylacrylamide (DMA, 9.92 g, 0.100 mol), t-amyl alcohol (96.63 g), a polymerization initiator VA-061 (Wako Pure Chemical Industries, Ltd., 0.0310 g, 0.124 mmol), 2-mercaptoethanol (86 μL, 1.23 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 (=400 mL/30 mL, 500 mL/40 mL, 130 mL/3 mL and 200 mL/7 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: 4.3 kD, Mw: 17 kD (Mw/Mn=4.1)).

후처리

  1. customequipped with a three-way
  2. customAfter degassing inside the three-necked flask
  3. customfollowed by temperature rise to 75° C.
  4. stirringfurther stirring for 4 hours
  5. customAfter completion of the polymerization
  6. customthe polymerization reaction solution
  7. distillationthe solvent was distilled off by an evaporator
  8. washwashed once with each of n-hexane/methanol (=400 mL/30 mL, 500 mL/40 mL, 130 mL/3 mL and 200 mL/7 mL)
  9. customThe solid component was dried overnight by a vacuum
  10. customdrying oven at 60° C
  11. additionLiquid nitrogen was charged
  12. customthe solid component was crushed by a spatula
  13. customdried by a vacuum
  14. customdrying oven at 60° C. for 3 hours

출처 및 근거

ORD 기록
ord-895378ea81a1413d9f958522f70f68b1
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09297930B2

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