2-Methylbenzenesulfonic acid → HCID 18326000、化合物

HRID 399884

反応式

HRID 399884 の反応式
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]

参加物

7

反応物 4

HCID 69252-Methylbenzenesulfonic acidHCID 12974Methacrylic anhydrideHCID 13719873HCID 13719873、化合物HCID 53950183HCID 53950183、化合物

生成物 1

HCID 18326000HCID 18326000、化合物

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 1140Toluene溶媒2 回

反応条件

温度
100 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6b267d8fecba4701972798274e4568d9
出典データセット
uspto-grants-1998_10
特許番号
US05824733

関連ノート

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