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Hydrochloric Acid → 2-tert-Butyl-6-(3-tert-butyl-2-hydroxy-5-methylbenzyl)-4-methylphenyl acrylate

HRID 638674
ノート
印刷プレビュー

反応式

HRID 638674 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](Cl)(=[O:29])[CH:27]=[CH2:28].Cl>C(N(CC)CC)C.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:29])[CH:27]=[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 3

HCID 313Hydrochloric AcidHCID 83982,2'-Methylenebis(4-methyl-6-tert-butylphenol)HCID 13140Acryloyl chloride

生成物 1

HCID 1090582-tert-Butyl-6-(3-tert-butyl-2-hydroxy-5-methylbenzyl)-4-methylphenyl acrylate収率 94.7%

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒
HCID 8471
Triethylamine
溶媒
2 回

実験手順

To a 500-ml four-necked flask equipped with a thermometer, stirring apparatus, condenser and dropping funnel were added 82.0 g (0.241 mole) of 2,2'-methylenebis(6-tert-butyl-4-methylphenol), 200 g of toluene and 23.9 g (0.290 mole) of triethylamine. After replacing the air in the container with nitrogen, 25 g (0.276 mole) of acryloyl chloride was added dropwise with stirring. After completion of the dropwise addition, stirring was continued for 1 hour, excess triethylamine was neutralized with a dilute hydrochloric acid and the formed triethylamine hydrochloride was then removed by washing with water. Toluene was then removed by evaporation from the toluene layer after completion of the washing, and the residue obtained was recrystallized from 20 g of n-hexane to obtain 90.0 g of 2,2'-methylenebis(6-tert-butyl-4-methylphenol) monoacrylate as a white crystal. Melting point, 132°-134° C. Yield, 95%.

後処理

  1. customTo a 500-ml four-necked flask equipped with a thermometer
  2. additionwas added dropwise
  3. stirringwith stirring
  4. additionAfter completion of the dropwise addition
  5. stirringstirring
  6. customthe formed triethylamine hydrochloride was then removed
  7. washby washing with water
  8. customToluene was then removed by evaporation from the toluene layer after completion of the washing
  9. customthe residue obtained
  10. customwas recrystallized from 20 g of n-hexane

出典と根拠

ORDレコード
ord-5c626098b6624ff5ab4929555e564683
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

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