Acetyl chloride → 2-methyl-4-acetyl-1-naphthol

HRID 234097

반응식

HRID 234097 반응식
[CH3:1][C:2]1[CH:11]=[CH:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:3]=1[OH:12].[Cl-].[Al+3].[Cl-].[Cl-].[C:17](Cl)(=[O:19])[CH3:18]>ClCCl>[CH3:1][C:2]1[CH:11]=[C:10]([C:17](=[O:19])[CH3:18])[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:3]=1[OH:12]

참가 물질

5

반응물 3

HCID 6367Acetyl chlorideHCID 240552-Methyl-1-naphtholHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 109655292-methyl-4-acetyl-1-naphthol

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To an ice-cooled solution of 2-methyl-l-naphthol (7.9 g, 0.05 mmol) in dichloromethane, anhydrous aluminum chloride (7.2 g) was slowly added with stirring, followed by slow addition of acetyl chloride (4.7 g) to start reaction. The reaction mixture was stirred at 10° C. or below for 1 h, then at room temperature for 3 h. Thereafter, the mixture was poured into ice water. Then, the reaction product was extracted with dichloromethane and the extracted layer was washed with water. Further, the extracted layer was dried over anhydrous sodium sulfate and the solvent was distilled off under reduced pressure. The residue was recrystallized with benzene, giving the desired compound, 2-methyl-4-acetyl-l-naphthol, in an amount of 3.9 g.

후처리

  1. additionwas slowly added
  2. customreaction
  3. stirringThe reaction mixture was stirred at 10° C. or below for 1 h
  4. extractionThen, the reaction product was extracted with dichloromethane
  5. washthe extracted layer was washed with water
  6. dry with materialFurther, the extracted layer was dried over anhydrous sodium sulfate
  7. distillationthe solvent was distilled off under reduced pressure
  8. customThe residue was recrystallized with benzene

출처 및 근거

ORD 기록
ord-573178efefc6497e887c708f1cc20aa1
출처 데이터셋
uspto-grants-1997_01
특허 번호
US05594112

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