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p-Toluenesulfonic acid → Acrylic acid 3,3,4,4-tetrafluoro-4-heptafluoropropyloxy-butyl ester

HRID 557478
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HRID 557478 반응식
[C:1]([OH:5])(=[O:4])[CH:2]=[CH2:3].[F:6][C:7]([F:25])([C:21]([F:24])([F:23])[F:22])[C:8]([F:20])([F:19])[O:9][C:10]([F:18])([F:17])[C:11]([F:16])([F:15])[CH2:12][CH2:13]O.C1(C)C=CC(S(O)(=O)=O)=CC=1>>[F:15][C:11]([F:16])([C:10]([F:17])([F:18])[O:9][C:8]([F:19])([F:20])[C:7]([F:6])([F:25])[C:21]([F:22])([F:24])[F:23])[CH2:12][CH2:13][O:4][C:1](=[O:5])[CH:2]=[CH2:3]
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4

반응물 3

HCID 6101p-Toluenesulfonic acidHCID 6581Acrylic AcidHCID 577405752-[2-(Heptafluoropropoxy)-tetrafluoroethyl]-ethyl alcohol

생성물 1

HCID 86631012Acrylic acid 3,3,4,4-tetrafluoro-4-heptafluoropropyloxy-butyl ester

실험 절차

Acrylic acid was esterified with 2-[2-(heptafluoropropoxy)-tetrafluoroethyl]-ethyl alcohol (US 2008113199 A1) in the presence catalytic amounts of p-toluene sulfonic acid to yield acrylic acid 3,3,4,4-tetrafluoro-4-heptafluoropropyloxy-butyl ester quantitatively. The ester was washed with water and distilled prior to the reaction with APTES (Aminopropyl triethoxysilane, CAS#919-30-2). A solution of one equivalent of APTES and two equivalents acrylic acid 3,3,4,4-tetrafluoro-4-heptafluoropropyloxy-butyl in absolute ethanol were allowed to stir at 60° C. for 5 h. The solvent was distilled of under reduced pressure to provide the desired twin-tail silane (tertiary amine fluorosilane) quantitatively as a colorless oil.

출처 및 근거

ORD 기록
ord-2ea0057a792c48289b1017ce5d390b31
출처 데이터셋
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08058463B2

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