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Hydrogen Peroxide → 4-(3-Bromophenyl)butan-1-ol

HRID 573921
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HRID 573921 반응식
[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH2:8][CH2:9][CH:10]=[CH2:11])[CH:3]=1.[OH-:12].[Na+].OO>>[Br:1][C:2]1[CH:3]=[C:4]([CH2:8][CH2:9][CH2:10][CH2:11][OH:12])[CH:5]=[CH:6][CH:7]=1
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참가 물질

4

반응물 3

HCID 784Hydrogen PeroxideHCID 14798Sodium HydroxideHCID 157251651-Bromo-3-(but-3-en-1-yl)benzene

생성물 1

HCID 218954894-(3-Bromophenyl)butan-1-ol수율 92%

실험 절차

To a solution of 1-bromo-3-(but-3-en-1-yl)benzene (CA46) (7.51 g, 35.6 mmol) in hexanes (80 mL) was added (1S,5S)-9-borabicyclo[3.3.1]nonane (0.5 M in tetrahydrofuran, 74.7 mL, 37.4 mmol). The reaction was allowed to stir at room temperature overnight. To the resulting clear solution sodium hydroxide (6.0 M, 5.93 mL, 35.6 mmol) was added dropwise. The reaction was placed in an ice water bath and hydrogen peroxide (13.8 mL, 135 mmol) was added. The resulting mixture was then heated to an internal temperature of 50° C. for overnight. The reaction mixture was cooled to room temperature. The biphasic solution was partitioned, and the organic layer was washed with sodium bisulfite, and brine solution. The combined aqueous layers were made basic with saturated sodium carbonate, and extracted with diethyl ether (2×100 mL). The combined organics were dried over magnesium sulfate, filtered, and concentrated. The liquid was loaded on to silica and purified by flash column chromatography using 0-40% ethyl acetate/hexanes as eluent providing the title compound as a clear liquid (7.50 g, 90%): 1H NMR (400 MHz, DMSO-d6) δ 7.40 (t, J=1.9 Hz, 1H), 7.37 (dt, J=7.6, 1.8 Hz, 1H), 7.28-7.17 (m, 2H), 4.39 (t, J=5.2 Hz, 1H), 3.40 (td, J=6.5, 5.2 Hz, 2H), 2.57 (t, J=7.6 Hz, 2H), 1.65-1.51 (m, 2H), 1.49-1.35 (m, 2H); EIMS m/z 228 ([M]+).

후처리

  1. customThe reaction was placed in an ice water bath
  2. temperatureThe resulting mixture was then heated to an internal temperature of 50° C. for overnight
  3. temperatureThe reaction mixture was cooled to room temperature
  4. customThe biphasic solution was partitioned
  5. washthe organic layer was washed with sodium bisulfite, and brine solution
  6. extractionextracted with diethyl ether (2×100 mL)
  7. dry with materialThe combined organics were dried over magnesium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated
  10. custompurified by flash column chromatography

출처 및 근거

ORD 기록
ord-0ecef67026c74bf99b94c876ad0172df
출처 데이터셋
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09029560B2

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