Ethyl Acetate → MAU 2,2,2-trifluoroethyl acrylate

HRID 405655

反応式

HRID 405655 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:24][CH2:25][C:26]([F:29])([F:28])[F:27])(=[O:23])[CH:21]=[CH2:22].C(OCC)(=O)C>CO>[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:24][CH2:25][C:26]([F:29])([F:28])[F:27])(=[O:23])[CH:21]=[CH2:22]

参加物

5

反応物 3

HCID 8857Ethyl AcetateHCID 678892,2,2-Trifluoroethyl acrylateHCID 276418511-(Methacryloylamino)undecanoic acid

生成物 1

HCID 131731614MAU 2,2,2-trifluoroethyl acrylate収率 274.5%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
60 °C

実験手順

In 59.68 g of methanol were dissolved 18.80 g (69.82 mmol) of 11-methacrylamidoundecanoic acid (MAU), 1.20 g (7.76 mmol) of 2,2,2-trifluoroethyl acrylate (Tokyo Chemical industry Co.), and 0.32 g (1.95 mmol) of azoloisisobutyronitrile (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, 9.02 g of random MAU/2,2,2-trifluoroethyl acrylate copolymer (90/10) was obtained (yield: 45.1%). The weight average molecular weight was 35000.

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-618c7b21dc874207bacd3ca366a97352
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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