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Acetone → 1-Bromo-3-(4-chlorophenyl)propan-2-one

HRID 2402043
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HRID 2402043 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9](=[O:11])[CH3:10])=[CH:4][CH:3]=1.[BrH:12].BrBr.CC(C)=O>C(O)(=O)C>[Br:12][CH2:10][C:9](=[O:11])[CH2:8][C:5]1[CH:4]=[CH:3][C:2]([Cl:1])=[CH:7][CH:6]=1
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참가 물질

6

반응물 4

HCID 180AcetoneHCID 260Hydrogen BromideHCID 24408BromineHCID 796991-(p-Chlorophenyl)acetone

생성물 1

HCID 147488551-Bromo-3-(4-chlorophenyl)propan-2-one수율 69.3%

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

실험 절차

To a solution of 1-(4-chlorophenyl)propan-2-one (25.0 g, 148 mmol) in acetic acid (37.9 mL) was added 48% aqueous HBr (19.0 mL, 168 mmol). A solution of bromine (16.3 mL, 316 mmol) in acetic acid (63.2 mL) was then added over 10 minutes and the resulting solution was stirred for 4 hours at room temperature. Acetone (190 mL) was added and the resulting solution was stirred at room temperature for 3 days. The reaction was concentrated in vacuo and the residue was taken up in DCM (300 mL) and brine (100 mL). The layers were separated and the aqueous layer was extracted with DCM (100 mL). The combined organic layers were dried over MgSO4, filtered, and concentrated in vacuo. The residue was purified by silica gel chromatography (ethyl acetate/hexanes=0/100→15/85) to give 25.4 grams of the title compound as a dark gray solid (69% yield). 1H NMR (400 MHz, CDCl3) δ: 7.34-7.31 (m, 2H), 7.18-7.15 (m, 2H), 3.94 (s, 2H), 3.91 (2, 2H).

후처리

  1. stirringthe resulting solution was stirred at room temperature for 3 days
  2. concentrationThe reaction was concentrated in vacuo
  3. customThe layers were separated
  4. extractionthe aqueous layer was extracted with DCM (100 mL)
  5. dry with materialThe combined organic layers were dried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. customThe residue was purified by silica gel chromatography (ethyl acetate/hexanes=0/100→15/85)

출처 및 근거

ORD 기록
ord-6d1b2e5cdb97479db93cdb6918703025
출처 데이터셋
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08796271B2

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