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Methacrylic Acid → 2-Propenoic acid, 2-methyl-, 2-(1,1-dimethylethyl)-6-((3-(1,1-dimethylethyl)-2-hydroxy-5-methylphenyl)methyl)-4-methylphenyl ester

HRID 638670
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HRID 638670 반응식
[CH2:1]([C:14]1[CH:19]=[C:18]([CH3:20])[CH:17]=[C:16]([C:21]([CH3:24])([CH3:23])[CH3:22])[C:15]=1[OH:25])[C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[C:4]([C:9]([CH3:12])([CH3:11])[CH3:10])[C:3]=1[OH:13].[C:26](O)(=[O:30])[C:27]([CH3:29])=[CH2:28].C(N(CC)CC)C.C1(C)C(S(Cl)(=O)=O)=CC=CC=1>C1(C)C=CC=CC=1>[C:26]([O:25][C:15]1[C:16]([C:21]([CH3:24])([CH3:23])[CH3:22])=[CH:17][C:18]([CH3:20])=[CH:19][C:14]=1[CH2:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[C:4]([C:9]([CH3:12])([CH3:11])[CH3:10])[C:3]=1[OH:13])(=[O:30])[C:27]([CH3:29])=[CH2:28]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 4093Methacrylic AcidHCID 83982,2'-Methylenebis(4-methyl-6-tert-butylphenol)HCID 8471TriethylamineHCID 8623o-Toluenesulfonyl chloride

생성물 1

HCID 1090592-Propenoic acid, 2-methyl-, 2-(1,1-dimethylethyl)-6-((3-(1,1-dimethylethyl)-2-hydroxy-5-methylphenyl)methyl)-4-methylphenyl ester수율 94%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

To the same flask as used in Example 1 were added 340.51 g (1.0 mole) of 2,2'-methylenebis(6-tert-butyl-4-methylphenol), 86.41 g (1.0 mole) of 98.5% methacrylic acid, 500 g of toluene and 242.86 g (2.4 moles) of triethylamine. After replacing the air in the container with nitrogen, 229.14 g (1.2 moles) of o-toluenesulfonyl chloride was added dropwise with stirring. After completion of the dropwise addition, the reaction solution was kept at 90° C. for 1 hour. Thereafter, the organic layer was washed with water until it became neutral, and toluene was removed under reduced pressure. The residue was recrystallized from n-hexane to obtain 384.1 g of a white crystalline 2,2'-methylenebis(6-tert-butyl-4-methylphenol) monomethacrylate having a melting point of 144° to 146° C. Yield, 94%.

후처리

  1. additionwas added dropwise
  2. additionAfter completion of the dropwise addition
  3. washThereafter, the organic layer was washed with water until it
  4. customtoluene was removed under reduced pressure
  5. customThe residue was recrystallized from n-hexane

출처 및 근거

ORD 기록
ord-e686fe4dc07544349c8f09239672c13b
출처 데이터셋
uspto-grants-1985_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04562281

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