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Methanol → NaMAU AMPS

HRID 405652
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HRID 405652 반응식
CO.[C:3]([NH:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][C:19]([O-:21])=[O:20])(=[O:7])[C:4]([CH3:6])=[CH2:5].[Na+:22].[C:23]([NH:27][C:28]([CH3:35])([CH3:34])[CH2:29][S:30]([OH:33])(=[O:32])=[O:31])(=[O:26])[CH:24]=[CH2:25].[OH-].[Na+]>N(C(C)(C)C#N)=NC(C)(C)C#N.CCOCC.O>[C:3]([NH:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][C:19]([O-:21])=[O:20])(=[O:7])[C:4]([CH3:6])=[CH2:5].[Na+:22].[C:23]([NH:27][C:28]([CH3:35])([CH3:34])[CH2:29][S:30]([OH:33])(=[O:31])=[O:32])(=[O:26])[CH:24]=[CH2:25]
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참가 물질

8

반응물 4

HCID 887MethanolHCID 14798Sodium HydroxideHCID 653602-Acrylamido-2-methyl-1-propanesulfonic acidHCID 87229187Sodium 11-methacrylamidoundecanoate

생성물 1

HCID 131731611NaMAU AMPS수율 619.5%

시약·촉매·용매 3

HCID 6547
Azobisisobutyronitrile
촉매
HCID 962Water용매
HCID 3283Diethyl Ether용매

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온도
60 °C

실험 절차

Into a mixed solvent of 32.4 mL of methanol and 3.6 mL water (methanol/water=9/1) were dissolved 4.9823 g (17.1 mmol) of sodium 11-methacrylamidoundecanoate (NaMAU), 186.5 mg (0.9 mmol) of 2-acrylamido-2-methylpropanesulfonic acid (AMPS), 39.6 mg (0.99 mmol) of sodium hydroxide, and 7.4 mg (0.045 mmol) of azobisisobutyronitrile. The solution was deaerated by bubbling argon for 30 minutes, the container was covered with a septum, and the polymerization was conducted by heating the solution at 60° C. for 12 hours. After the completion of the polymerization reaction, the reaction solution was dropwise added into a large excess of ether, and the resulting precipitate was collected by filtration under suction. This precipitate was dissolved in water, dialyzed against pure water for 1 week, and 2.78 g of random NaMAU/AMPS copolymer (95/5) was obtained by freeze-drying (yield: 53.71%).

후처리

  1. customby bubbling argon for 30 minutes
  2. customAfter the completion of the polymerization reaction
  3. filtrationthe resulting precipitate was collected by filtration under suction
  4. dissolutionThis precipitate was dissolved in water
  5. customdialyzed against pure water for 1 week

출처 및 근거

ORD 기록
ord-e74563a5dfd343de944fdb3e46ef7ccc
출처 데이터셋
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08753686B2

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