Acetone → MAU N,N-dimethylaminoethyl acrylate methyl chloride

HRID 405660

반응식

HRID 405660 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].[CH3:20][Cl:21].[C:22]([O:26][CH2:27][CH2:28][N:29]([CH3:31])[CH3:30])(=[O:25])[CH:23]=[CH2:24].CC(C)=O>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].[CH3:20][Cl:21].[C:22]([O:26][CH2:27][CH2:28][N:29]([CH3:31])[CH3:30])(=[O:25])[CH:23]=[CH2:24]

참가 물질

6

반응물 3

HCID 180AcetoneHCID 276418511-(Methacryloylamino)undecanoic acidHCID 22395581Dimethylaminoethyl acrylate methylchloride

생성물 1

HCID 131731619MAU N,N-dimethylaminoethyl acrylate methyl chloride수율 266.6%

시약·촉매·용매 2

HCID 6547Azobisisobutyronitrile촉매HCID 887Methanol용매

반응 조건

온도
60 °C

실험 절차

In 59.69 g of methanol were dissolved 18.52 g (68.77 mmol) of 11-methacrylamidoundecanoic acid (MAU), 1.48 g (7.64 mmol) of N,N-dimethylaminoethyl acrylate methyl chloride (Kohjin Co., Ltd.), 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 obtained solution was dropwise added into a large excess of acetone, and the resulting precipitate was collected by filtration under suction. After drying under reduced pressure, 9.43 g of random MAU/N,N-dimethylaminoethyl acrylate methyl chloride copolymer (90/10) was obtained (yield: 47.2%). The weight average molecular weight was 68000.

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-d3c3d716cd464371a9eb4951320aa495
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08753686B2

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