Ethyl Acetate → MAU potassium 3-methacryloxypropanesulfonate

HRID 405653

반응식

HRID 405653 반응식
[C:1]([NH:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][C:17]([OH:19])=[O:18])(=[O:5])[C:2]([CH3:4])=[CH2:3].[C:20]([O:25][CH2:26][CH2:27][CH2:28][S:29]([O-:32])(=[O:31])=[O:30])(=[O:24])[C:21]([CH3:23])=[CH2:22].[K+:33].C(OCC)(=O)C>CO.N(C(C)(C)C#N)=NC(C)(C)C#N>[C:1]([NH:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][C:17]([OH:19])=[O:18])(=[O:5])[C:2]([CH3:4])=[CH2:3].[C:20]([O:25][CH2:26][CH2:27][CH2:28][S:29]([O-:32])(=[O:30])=[O:31])(=[O:24])[C:21]([CH3:23])=[CH2:22].[K+:33]

참가 물질

6

반응물 3

HCID 8857Ethyl AcetateHCID 276418511-(Methacryloylamino)undecanoic acidHCID 23682747Potasium 3-sulphopropyl methacrylate

생성물 1

HCID 131731612MAU potassium 3-methacryloxypropanesulfonate수율 478.2%

시약·촉매·용매 2

HCID 6547Azobisisobutyronitrile촉매HCID 887Methanol용매

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온도
60 °C

실험 절차

In 59.69 g of methanol were dissolved 18.15 g (67.41 mmol) of 11-methacrylamidoundecanoic acid (MAU), 1.85 g (7.49 mmol) of potassium 3-methacryloxypropanesulfonate (Tokyo Chemical industry Co.), and 0.31 g (1.89 mmol) of azobisisobutyronitrile (Nacalai Tesque, Inc.). The solution was deaerated by bubbling nitrogen for 60 minutes. The container was covered with a septum, and the polymerization was conducted by heating at 60° C. for 20 hours. After the completion of the polymerization reaction, the reaction solution was dropwise added into a large excess of ethyl acetate, and the resulting precipitate was collected by filtration under suction. After drying under reduced pressure, 18.47 g of random MAU/potassium 3-methacryloxypropanesulfonate copolymer (90/10) was obtained (yield: 92.4%). The weight average molecular weight was 240000.

후처리

  1. customby bubbling nitrogen for 60 minutes
  2. customAfter the completion of the polymerization reaction
  3. filtrationthe resulting precipitate was collected by filtration under suction
  4. customAfter drying under reduced pressure

출처 및 근거

ORD 기록
ord-afe1d64d88df42dfb71c051d1640df24
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08753686B2

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