Ethyl Acetate → MAU potassium 3-methacryloxypropanesulfonate

HRID 405653

反応式

HRID 405653 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].[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]

参加物

6

反応物 3

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

生成物 1

HCID 131731612MAU potassium 3-methacryloxypropanesulfonate収率 478.2%

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 18.15 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.

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-afe1d64d88df42dfb71c051d1640df24
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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