Anisole → 1-(4-Methoxyphenyl)-3-methylbutan-1-one

HRID 732241노트

반응식

HRID 732241 반응식
[C:1](Cl)(=[O:6])[CH2:2][CH:3]([CH3:5])[CH3:4].[Cl-].[Al+3].[Cl-].[Cl-].[C:12]1([O:18][CH3:19])[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1>ClCCl>[CH3:19][O:18][C:12]1[CH:17]=[CH:16][C:15]([C:1](=[O:6])[CH2:2][CH:3]([CH3:5])[CH3:4])=[CH:14][CH:13]=1

참가 물질

5

반응물 3

HCID 7519AnisoleHCID 66054Isovaleryl chloride2회HCID 6451240Aluminum(III) Chloride

생성물 1

HCID 127577691-(4-Methoxyphenyl)-3-methylbutan-1-one수율 98.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

While 40 g of isovaleryl chloride and 44 g of aluminum chloride were added to 140 ml of dichloromethane and stirred, 32.6 ml of anisole were slowly added in droplets at −10° C. or lower, and stirring was continued at room temperature for 40 min. Subsequently, 36.6 ml of isovaleryl chloride were slowly added in droplets, and stirring was further continued at room temperature for 18 hr. After the reaction was completed, the resultant reaction mixture was added with 200 ml of dichloromethane, and then washed with a saturated aqueous solution of sodium bicarbonate and water, in that order, after which the dichloromethane layer was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure, thus obtaining 56.9 g (yield: 98.6%) of a title compound as light yellow liquid.

후처리

  1. stirringlower, and stirring
  2. stirringstirring
  3. waitwas further continued at room temperature for 18 hr
  4. customthe resultant reaction mixture
  5. washwashed with a saturated aqueous solution of sodium bicarbonate and water, in that order
  6. dry with materialafter which the dichloromethane layer was dried over anhydrous magnesium sulfate
  7. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-6128e92980404ec8aa0fe45313beb7b0
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07585979B2

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