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(Bis(2-methoxyethyl)amino)sulfur trifluoride → 4-Bromo-1-chloro-2-(1-fluoroethyl)benzene

HRID 245271
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HRID 245271 반응식
COCCN(S(F)(F)[F:11])CCOC.[Br:14][C:15]1[CH:16]=[CH:17][C:18]([Cl:24])=[C:19]([CH:21](O)[CH3:22])[CH:20]=1>ClCCl.O>[Br:14][C:15]1[CH:16]=[CH:17][C:18]([Cl:24])=[C:19]([CH:21]([F:11])[CH3:22])[CH:20]=1
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참가 물질

5

반응물 2

HCID 2734690(Bis(2-methoxyethyl)amino)sulfur trifluorideHCID 587626441-(5-Bromo-2-chlorophenyl)ethanol

생성물 1

HCID 591269474-Bromo-1-chloro-2-(1-fluoroethyl)benzene수율 65.8%

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매

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온도
0 °C

실험 절차

Bis(2-methoxyethyl)aminosulfur trifluoride (4.5 g, 20.34 mmol) was added to a stirred solution of 1-(5-bromo-2-chlorophenyl)ethanol (3.99 g, 16.95 mmol) in dichloromethane (50 mL) at 0° C. The resulting solution was stirred at 0° C. for 3 h. The reaction mixture was quenched with a 5% solution of aqueous sodium bicarbonate (100 mL) and the resulting bubbling biphasic reaction mixture was vigorously stirred at 0° C. for 15 min. The reaction mixture was diluted with water (50 mL) and extracted with dichloromethane twice. The combined organic layers were washed with 1M hydrochloric acid, dried and concentrated by rotary evaporation. The product was purified by flash chromatography on silica gel (hexanes) to yield the title compound (2.65 g, 11.16 mmol, 65.8% yield) as a clear oil: 1H NMR (CDCl3) δ 7.65 (d, 1H), 7.37 (m, 1H), 7.20 (m, 1H), 5.88 (dq, 1H), 1.61 (dd, 3H).

후처리

  1. customThe reaction mixture was quenched with a 5% solution of aqueous sodium bicarbonate (100 mL)
  2. customthe resulting bubbling
  3. custombiphasic reaction mixture
  4. stirringwas vigorously stirred at 0° C. for 15 min
  5. extractionextracted with dichloromethane twice
  6. washThe combined organic layers were washed with 1M hydrochloric acid
  7. customdried
  8. concentrationconcentrated by rotary evaporation
  9. customThe product was purified by flash chromatography on silica gel (hexanes)

출처 및 근거

ORD 기록
ord-a272d6206e164cd8bf2782c465e6bf64
출처 데이터셋
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08658791B2

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