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Hydrochloric Acid → 2-tert-Butyl-4-methylphenyl prop-2-enoate

HRID 1719349
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HRID 1719349 반응식
[C:1]([C:5]1[CH:10]=[C:9]([CH3:11])[CH:8]=[CH:7][C:6]=1[OH:12])([CH3:4])([CH3:3])[CH3:2].[C:13](Cl)(=[O:16])[CH:14]=[CH2:15].Cl>C(N(CC)CC)C.C1(C)C=CC=CC=1>[C:13]([O:12][C:6]1[CH:7]=[CH:8][C:9]([CH3:11])=[CH:10][C:5]=1[C:1]([CH3:4])([CH3:3])[CH3:2])(=[O:16])[CH:14]=[CH2:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 13140Acryloyl chlorideHCID 170042-tert-Butyl-4-methylphenol

생성물 1

HCID 202680562-tert-Butyl-4-methylphenyl prop-2-enoate

시약·촉매·용매 2

HCID 1140Toluene용매HCID 8471Triethylamine용매2회

실험 절차

To a 300-ml four-necked flask equipped with a thermometer, a stirrer, a condenser and a dropping funnel were added 32.8 g (0.20 mole) of 2-tert-butyl-4-methylphenol, 22.3 g (0.22 mole) of triethylamine and 100 g of toluene, and after replacing air in the flask by nitrogen, 19.10 g (0.21 mole) of acryloyl chloride was added dropwise at a reaction temperature of 30° C. over 1 hour. After completion of the dropwise addition, excessive triethylamine was neutralized with hydrochloric acid, the reaction solution was washed with water, and toluene was then removed from the organic layer by evaporation under reduced pressure to obtain 43.0 g of a crude product (yield, 99%). This crude product was purified by distillation under reduced pressure to obtain a white and transparent 2-tert-butyl-4-methylphenol monoacrylate.

후처리

  1. customTo a 300-ml four-necked flask equipped with a thermometer, a stirrer, a condenser and a dropping funnel
  2. additionwas added dropwise at a reaction temperature of 30° C. over 1 hour
  3. washthe reaction solution was washed with water, and toluene
  4. customwas then removed from the organic layer by evaporation under reduced pressure
  5. customto obtain 43.0 g of a crude product (yield, 99%)
  6. distillationThis crude product was purified by distillation under reduced pressure

출처 및 근거

ORD 기록
ord-824f1c3cfa8e48caaa2b8c9808dc05a3
출처 데이터셋
uspto-grants-1985_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04539355

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