Tetrabutylammonium → Methacrylic Acid

HRID 440427

반응식

HRID 440427 반응식
C[O:2][C:3]([O:7][Si](C)(C)C)=[C:4]([CH3:6])[CH3:5].C([N+](CCCC)(CCCC)CCCC)CCC.[C:29]([O:34][Si](C)(C)C)(=[O:33])[C:30]([CH3:32])=[CH2:31].C(O)(=O)C(C)=C.[CH2:45]([O:47][CH:48]([OH:57])[CH2:49][O:50][CH2:51][CH2:52][O:53][CH2:54][CH2:55][OH:56])[CH3:46].C(OCCC1C=CC=CC=1)(=O)C(C)=C.[F-].C([N+](CCCC)(CCCC)CCCC)CCC>C1(=O)OC(C)CO1.C1COCC1>[C:3]([OH:7])(=[O:2])[C:4]([CH3:6])=[CH2:5].[C:29]([OH:34])(=[O:33])[C:30]([CH3:32])=[CH2:31].[CH2:45]([O:47][CH:48]([OH:57])[CH2:49][O:50][CH2:51][CH2:52][O:53][CH2:54][CH2:55][OH:56])[CH3:46]

참가 물질

10

반응물 6

HCID 16028Tetrabutylammonium3회HCID 772602-Phenylethyl methacrylateHCID 552336Silane, ((1-methoxy-2-methyl-1-propenyl)oxy)trimethyl-HCID 2724141Tetrabutylammonium FluorideHCID 27338392-Propenoic acid, 2-methyl-, trimethylsilyl ester2회HCID 86746980b-Ethoxytriethylene glycol methacrylate2회

생성물 2

HCID 4093Methacrylic AcidHCID 86746980b-Ethoxytriethylene glycol methacrylate

시약·촉매·용매 2

HCID 7924Propylene Carbonate용매3회HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 2.53 g (2.93 mL, 14.5 mmol) of 1-methoxy-1-trimethylsiloxy-2-methyl-1-propene and 0.5 mL of tetrabutylammonium biacetate (0.1 M in propylene carbonate) in 40 mL of THF was added dropwise a mixture of 29.8 g (33.7 mL, 0.189 mole) of trimethylsilyl methacrylate and 14.5 g (14.5 mL, 0.0582 mole) of ethoxytriethylene glycol methacrylate. The temperature of the reaction mixture rose from 26° C. to 40° C. After addition of an additional 0.5 mL of tetrabutylammonium biacetate (0.1 M in propylene carbonate), the temperature rose to 57° C. When the temperature had fallen to 29° C., 0.3 mL of tetrabutylammonium biacetate (0.1 M in propylene carbonate) was added, followed by 29.9 g (29.6 mL, 0. 157 mole) of 2-phenylethyl methacrylate. The temperature rose to 48° C., and the mixture was stirred overnight. NMR analysis of an aliquot of the reaction mixture showed that there was no residual monomer in the solution of poly(trimethylsilyl methacrylate [46.8 mol %]-co-ethoxytriethylene glycol methacrylate [14.4 mol %]-b-2-phenylethyl methacrylate [38.8 mol %]). The solution was treated with 45 mL of tetrabutylammonium fluoride (0.03 M in methanol) and stirred at reflux for 8 hr. Evaporation under reduced pressure followed by drying in a vacuum oven gave 66.5 g of poly(methacrylic acid [46.8 mol %]-co-ethoxytriethylene glycol methacrylate [14.4 mol %]-b-2-phenylethyl methacrylate [38.8 mol %]).

후처리

  1. customrose from 26° C. to 40° C
  2. customrose to 57° C
  3. customhad fallen to 29° C.
  4. customrose to 48° C.
  5. stirringstirred
  6. temperatureat reflux for 8 hr
  7. customEvaporation under reduced pressure
  8. customby drying in a vacuum oven

출처 및 근거

ORD 기록
ord-4fc62329022d455abcec9f27fd304b9c
출처 데이터셋
uspto-grants-1996_05
특허 번호
US05519085

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