Hydrochloric Acid → 3',5'-Bis(tert-butyl)-4'-hydroxyacetophenone

HRID 2947

반응식

HRID 2947 반응식
[C:1](Cl)(=[O:3])[CH3:2].[C:5]([C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([C:15]([CH3:18])([CH3:17])[CH3:16])[C:10]=1[OH:19])([CH3:8])([CH3:7])[CH3:6].Cl>C(Cl)Cl>[CH3:16][C:15]([C:11]1[CH:12]=[C:13]([C:1](=[O:3])[CH3:2])[CH:14]=[C:9]([C:5]([CH3:8])([CH3:7])[CH3:6])[C:10]=1[OH:19])([CH3:18])[CH3:17]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 6367Acetyl chlorideHCID 314052,6-Di-tert-butylphenol

생성물 1

HCID 6162963',5'-Bis(tert-butyl)-4'-hydroxyacetophenone

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
-4 °C

실험 절차

Under a nitrogen atmosphere, 6.89 ml of acetylchloride and 14.75 ml of stannic chloride were dissolved in 200 ml of methylene chloride and chilled to -4° C. To this was added 20 g of 2,6-di-t-butylphenol (in 100 ml of methylene chloride) over 10 minutes. The resultant mixture was stirred for 30 minutes at 0° C., then poured into a mixture of 400 ml of ice and 1N hydrochloric acid and stirred. The mixture separated into layers which were subsequently separated. The organic layer was washed with 100 ml of saturated sodium bicarbonate and 100 ml of brine. The organic layer was dried and the solvent evaporated to give 23.39 g of the desired subtitled intermediate.

후처리

  1. customThe mixture separated into layers which
  2. customwere subsequently separated
  3. washThe organic layer was washed with 100 ml of saturated sodium bicarbonate and 100 ml of brine
  4. customThe organic layer was dried
  5. customthe solvent evaporated

출처 및 근거

ORD 기록
ord-5ea8ac69bd1848ae813a64e74a7a7adf
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05731336

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