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Aluminum(III) Chloride → HCID 22172947, 화합물

HRID 716455
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HRID 716455 반응식
[Al+3].[Cl-].[Cl-].[Cl-].[Br:5][C:6]1[CH:7]=[CH:8][C:9]([CH3:18])=[C:10]([CH2:12][CH:13]([CH3:17])[C:14](Cl)=[O:15])[CH:11]=1>ClCCl>[Br:5][C:6]1[CH:7]=[CH:8][C:9]([CH3:18])=[C:10]2[C:11]=1[C:14](=[O:15])[CH:13]([CH3:17])[CH2:12]2
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참가 물질

4

반응물 2

HCID 6451240Aluminum(III) ChlorideHCID 89392410HCID 89392410, 화합물

생성물 1

HCID 22172947HCID 22172947, 화합물수율 99.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a stirred suspension of 49.5 g (0.371 mol, 1.2 eq.) of AlCl3 in 300 ml of dichloromethane a solution of 85.3 g (0.310 mol) of 3-(5-bromo-2-methylphenyl)-2-methylpropanoyl chloride in 50 ml of dichloromethane was added dropwise. This mixture was stirred overnight at room temperature and then poured on 500 g of ice. The organic layer was separated, and the aqueous layer was additionally extracted with 3×75 ml of dichloromethane. The combined organic extract was washed by aqueous K2CO3, dried over K2CO3, passed through a short pad of silica gel, and then evaporated to dryness. This procedure gave 74.0 g (>99%) of 7-bromo-2,4-dimethylindan-1-one as a light-orange liquid, solidified at room temperature, which was further used without an additional purification.

후처리

  1. additionwas added dropwise
  2. customThe organic layer was separated
  3. extractionthe aqueous layer was additionally extracted with 3×75 ml of dichloromethane
  4. extractionThe combined organic extract
  5. washwas washed by aqueous K2CO3
  6. dry with materialdried over K2CO3
  7. customevaporated to dryness

출처 및 근거

ORD 기록
ord-48aa8145633b4c919197a4210979fdaa
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09187583B2

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