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

HRID 405655

반응식

HRID 405655 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 131731614MAU 2,2,2-trifluoroethyl acrylate수율 274.5%

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
60 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-618c7b21dc874207bacd3ca366a97352
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08753686B2

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