Acetone → MAU N,N-dimethylaminopropylacrylamide methyl chloride

HRID 405661

反応式

HRID 405661 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].[CH3:22][NH:23][N:24]([NH:32][CH3:33])[C:25](=[O:31])[C:26]([CH2:28][CH2:29][CH3:30])=[CH2:27].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].[CH3:22][NH:23][N:24]([NH:32][CH3:33])[C:25](=[O:31])[C:26]([CH2:28][CH2:29][CH3:30])=[CH2:27]

参加物

6

反応物 3

HCID 180AcetoneHCID 276418511-(Methacryloylamino)undecanoic acidHCID 131731621n,n-Dimethylaminopropylacrylamide methyl chloride

生成物 1

HCID 131731620MAU N,N-dimethylaminopropylacrylamide methyl chloride収率 257.2%

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 18.43 g (68.43 mmol) of 11-methacrylamidoundecanoic acid (MAU), 1.57 g (7.60 mmol) of N,N-dimethylaminopropylacrylamide 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, 9.60 g of random MAU/N,N-dimethylaminopropylacrylamide methyl chloride copolymer (90/10) was obtained (yield: 48.0%). The weight average molecular weight was 42000.

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-68e46679b516439bb09a5181474dc5c2
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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