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Bromine → 1-(4-Bromothiophen-2-yl)-2-methylpropan-1-one

HRID 656105
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HRID 656105 반응식
[CH3:1][CH:2]([CH3:10])[C:3]([C:5]1[S:6][CH:7]=[CH:8][CH:9]=1)=[O:4].[Cl-].[Al+3].[Cl-].[Cl-].[Br:15]Br>C(Cl)(Cl)Cl>[Br:15][C:8]1[CH:9]=[C:5]([C:3](=[O:4])[CH:2]([CH3:10])[CH3:1])[S:6][CH:7]=1
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참가 물질

5

반응물 3

HCID 24408BromineHCID 38624802-Methyl-1-(thiophen-2-yl)propan-1-oneHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 593327031-(4-Bromothiophen-2-yl)-2-methylpropan-1-one수율 40%

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

2-methyl-1-(2-thienyl)-1-propanone (2.3 g, 15 mmol) was diluted in chloroform (10 mL), and aluminum chloride (4.5 g, 34 mmol, 2.3 eq) was added. Bromine (0.82 mL, 16 mmol, 1.1 eq) was added as a solution in chloroform (15 mL), and the mixture was stirred at rt over the weekend. The crude reaction mixture was carefully poured onto ice water, then extracted with chloroform. The combined organics were dried over sodium sulfate, filtered, and concentrated to afford brown oil. The crude was purified by isco combiflash to give the title compound as brown oil (1.28 g, 40%).

후처리

  1. customThe crude reaction mixture
  2. additionwas carefully poured onto ice water
  3. extractionextracted with chloroform
  4. dry with materialThe combined organics were dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customto afford brown oil
  8. customThe crude was purified by isco combiflash

출처 및 근거

ORD 기록
ord-6e82853107d04ec6ae5b57c01e3c76bc
출처 데이터셋
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08071584B2

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