Acetone → MAU N,N-dimethylaminoethyl acrylate methyl chloride

HRID 405660

反応式

HRID 405660 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

HCID 131731619MAU N,N-dimethylaminoethyl acrylate methyl chloride収率 266.6%

試薬・触媒・溶媒 2

HCID 6547Azobisisobutyronitrile触媒HCID 887Methanol溶媒

反応条件

温度
60 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d3c3d716cd464371a9eb4951320aa495
出典データセット
uspto-grants-2014_06
特許番号
US08753686B2

関連ノート

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