Diethyl Ether → MAU 2,2,3,3-tetrafluoropropyl methacrylate

HRID 405656

反応式

HRID 405656 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][C:27]([F:32])([F:31])[CH:28]([F:30])[F:29])(=[O:24])[C:21]([CH3:23])=[CH2:22].C(OCC)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][C:27]([F:31])([F:32])[CH:28]([F:29])[F:30])(=[O:24])[C:21]([CH3:23])=[CH2:22]

参加物

6

反応物 3

HCID 3283Diethyl EtherHCID 1235152,2,3,3-Tetrafluoropropyl methacrylateHCID 276418511-(Methacryloylamino)undecanoic acid

生成物 1

HCID 131731615MAU 2,2,3,3-tetrafluoropropyl methacrylate収率 451.4%

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 18.47 g (68.60 mmol) of 11-methacrylamidoundecanoic acid (MAU), 1.53 g (7.62 mmol) of 2,2,3,3-tetrafluoropropyl methacrylate (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 diethyl ether, and the resulting precipitate was collected by filtration under suction. After drying under reduced pressure, 16.15 g of random MAU/2,2,3,3-tetrafluoropropyl methacrylate copolymer (90/10) was obtained (yield: 80.8%). The weight average molecular weight was 220000.

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-9dd40ec1c474402fb4e16fb3cddbbf5d
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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