2-Methylbenzenesulfonic acid → HCID 18326000, 화합물

HRID 399884

반응식

HRID 399884 반응식
C[Si](C)(C)O[C:4]1[CH:20]=[CH:19][C:7]([C:8]([O:10][C:11]2[CH:16]=[CH:15][C:14]([CH2:17][CH3:18])=[CH:13][CH:12]=2)=[O:9])=[CH:6][CH:5]=1.OC1C=[CH:39][C:27]([C:28]([O:30]C2C=CC(CC)=CC=2)=[O:29])=[CH:26]C=1.C(OC(=O)C(C)=C)(=O)C(C)=C.C1(C)C(S(O)(=O)=O)=CC=CC=1>C1(C)C=CC=CC=1.C(O)C>[C:28]([O:30][C:19]1[CH:20]=[CH:4][CH:5]=[CH:6][C:7]=1[C:8]([O:10][C:11]1[CH:16]=[CH:15][C:14]([CH2:17][CH3:18])=[CH:13][CH:12]=1)=[O:9])(=[O:29])[C:27]([CH3:39])=[CH2:26]

참가 물질

7

반응물 4

HCID 69252-Methylbenzenesulfonic acidHCID 12974Methacrylic anhydrideHCID 13719873HCID 13719873, 화합물HCID 53950183HCID 53950183, 화합물

생성물 1

HCID 18326000HCID 18326000, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매HCID 1140Toluene용매2회

반응 조건

온도
100 °C

실험 절차

A solution of 16.9 g of 4-ethylphenyl 4-trimethylsilyloxybenzoate (prepared according to the instructions in EP-A-0 358 205, page 9, section C) in 15 ml of toluene and 10 ml of ethanol was boiled under reflux for one hour and then freed from volatile constituents by heating at 100° C. for 60 minutes. The 13.3 g of 4-ethylphenyl 4-hydroxybenzoate which remained were dissolved, together with 30 g of methacrylic anhydride and 1.2 g of toluenesulfonic acid, in 15 ml of toluene and the solution was heated at 100° C. for 1 hour. After cooling, the product was precipitated with hexane and recrystallized from ethanol.

후처리

  1. temperatureunder reflux for one hour
  2. temperaturethe solution was heated at 100° C. for 1 hour
  3. temperatureAfter cooling
  4. customthe product was precipitated with hexane
  5. customrecrystallized from ethanol

출처 및 근거

ORD 기록
ord-6b267d8fecba4701972798274e4568d9
출처 데이터셋
uspto-grants-1998_10
특허 번호
US05824733

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