1-Chloro-4-(chloromethyl)benzene → 4-(4-Chlorophenyl)-3,3-dimethylbutan-2-one

HRID 978216노트

반응식

HRID 978216 반응식
[OH-].[K+].[Cl:3][C:4]1[CH:11]=[CH:10][C:7]([CH2:8]Cl)=[CH:6][CH:5]=1.[CH:12]([C:15]([CH3:17])=[O:16])([CH3:14])[CH3:13]>C1(C)C=CC=CC=1.[Br-].C([N+](CCCC)(CCCC)CCCC)CCC>[Cl:3][C:4]1[CH:11]=[CH:10][C:7]([CH2:8][C:12]([CH3:14])([CH3:13])[C:15](=[O:16])[CH3:17])=[CH:6][CH:5]=1

참가 물질

6

반응물 3

HCID 77231-Chloro-4-(chloromethyl)benzeneHCID 112513-Methyl-2-butanoneHCID 14797Potassium Hydroxide

생성물 1

HCID 128706324-(4-Chlorophenyl)-3,3-dimethylbutan-2-one수율 87%

시약·촉매·용매 2

HCID 74236Tetrabutylammonium Bromide촉매HCID 1140Toluene용매

반응 조건

온도
85 °C

실험 절차

254 g (4 mols) of powdered technical potassium hydroxide (88% pure) are suspended in 1 liter of toluene. To this are slowly added 40 g of tetrabutylammonium bromide and a mixture of 644 g (4 mols) of 4-chlorobenzyl chloride and 430 g (5 mols) of methyl isopropyl ketone at 85° C. The reaction mixture is stirred a further 3 hours at 85° C. and, after cooling down, it is filtered and the filtrate is washed to neutrality. 732.5 g (87% of theory) of 1-(4-chlorophenyl)-2,2-dimethyl-3-butanone of boiling point 87°-90° C./0.05 mbar are obtained by fractional distillation under high vacuum.

후처리

  1. temperatureafter cooling down
  2. filtrationit is filtered
  3. washthe filtrate is washed to neutrality

출처 및 근거

ORD 기록
ord-fdd0546fcb4d42b7aa24424df12ddef7
출처 데이터셋
uspto-grants-1987_05
특허 번호
US04663465

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