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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
ノート
印刷プレビュー

反応式

HRID 638670 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-e686fe4dc07544349c8f09239672c13b
出典データセット
uspto-grants-1985_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04562281

反応ノート

読み込み中…

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