Acetic Acid → 1,3,5-Trimethyl-2,4,6-tris(3,5-di-tert-butyl-4-hydroxybenzyl)benzene

HRID 1618360

反応式

HRID 1618360 の反応式
[C:1]([C:5]1[CH:10]=[C:9]([CH2:11]OC(=O)C)[CH:8]=[C:7]([C:16]([CH3:19])([CH3:18])[CH3:17])[C:6]=1[OH:20])([CH3:4])([CH3:3])[CH3:2].[C:21]1([CH3:29])[CH:26]=[C:25]([CH3:27])[CH:24]=[C:23]([CH3:28])[CH:22]=1.S(=O)(=O)(O)O.[C:35]([OH:38])(=O)[CH3:36]>>[CH3:29][C:21]1[C:26]([CH2:11][C:9]2[CH:10]=[C:5]([C:1]([CH3:3])([CH3:4])[CH3:2])[C:6]([OH:20])=[C:7]([C:16]([CH3:18])([CH3:19])[CH3:17])[CH:8]=2)=[C:25]([CH3:27])[C:24]([CH2:11][C:9]2[CH:10]=[C:5]([C:1]([CH3:4])([CH3:3])[CH3:2])[C:6]([OH:20])=[C:7]([C:16]([CH3:19])([CH3:18])[CH3:17])[CH:8]=2)=[C:23]([CH3:28])[C:22]=1[CH2:11][C:9]1[CH:10]=[C:36]([C:1]([CH3:2])([CH3:3])[CH3:4])[C:35]([OH:38])=[C:7]([C:16]([CH3:19])([CH3:17])[CH3:18])[CH:8]=1

参加物

5

反応物 4

HCID 176Acetic AcidHCID 1118Sulfuric AcidHCID 7947MesityleneHCID 84404Benzenemethanol, 3,5-bis(1,1-dimethylethyl)-4-hydroxy-, 1-acetate

生成物 1

HCID 743701,3,5-Trimethyl-2,4,6-tris(3,5-di-tert-butyl-4-hydroxybenzyl)benzene

反応条件

温度
60 °C

実験手順

To an acetic acid solution of 73 g of the thus produced product comprising 2,6-di-tert-butyl-4-acetoxymethylphenol (85.5% by GC) was added mesitylene (2.4 g) and sulfuric acid (2 g, 98%); the resulting solution was heated at 60° C. for six hours. Most of the acetic acid was removed under reduced pressure and 65-70° C.; the resulting paste was dissolved in heptane (120 g); and the resulting solution was washed with water (2×60 g) at 70-75° C. The solution was dried by azeotropic removal of water and cooled to ambient temperature; 1,3,5-trimethyl-2,4,6-tris(3,5-di-tert-butyl-4-hydroxybenzyl)benzene was isolated as an off-white solid (8.1 g).

後処理

  1. customMost of the acetic acid was removed under reduced pressure and 65-70° C.
  2. dissolutionthe resulting paste was dissolved in heptane (120 g)
  3. washand the resulting solution was washed with water (2×60 g) at 70-75° C
  4. dry with materialThe solution was dried by azeotropic removal of water
  5. temperaturecooled to ambient temperature

出典と根拠

ORDレコード
ord-6ecc0d52dc0e4f0d855c3a94d723519b
出典データセット
uspto-grants-2014_07
特許番号
US08766016B2

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