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4-Chlorophenol → Benzene, 1-bromo-3-(4-chlorophenoxy)-

HRID 52646
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HRID 52646 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[CH:4][CH:3]=1.C[O-].[Na+].[Br:12][C:13]1[CH:18]=[CH:17][CH:16]=[C:15](Br)[CH:14]=1>COCCOCCOC>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][C:15]2[CH:14]=[C:13]([Br:12])[CH:18]=[CH:17][CH:16]=2)=[CH:4][CH:3]=1
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참가 물질

5

반응물 3

HCID 46844-ChlorophenolHCID 79271,3-DibromobenzeneHCID 10942334Sodium Methoxide

생성물 1

HCID 10613003Benzene, 1-bromo-3-(4-chlorophenoxy)-수율 29.9%

시약·촉매·용매 1

HCID 8150Diglyme용매

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온도
165 °C

실험 절차

Under a nitrogen atmosphere, a solution of 13.6 grams (0.106 mole) of 4-chlorophenol in 50 mL of diglyme was stirred, and 24.1 mL (0.106 mole) of methanolic 25% sodium methoxide was added dropwise. Upon completion of addition, the reaction mixture was heated to about 165° C. to remove methanol. After the methanol was removed, the heating was ceased, and 25.0 grams (0.106 mole) of 1,3-dibromobenzene and 1.3 grams of cuprous bromide were added. Upon completion of the additions, the reaction mixture was heated to reflux where it was stirred for about 21 hours. The reaction mixture was then cooled and filtered. The filter cake was washed with diethyl ether, and the wash was combined with the filtrate. The combination was extracted with two 20 mL portions of aqueous 20% sodium hydroxide and then with two 75 mL portions of an aqueous solution saturated with sodium chloride. The organic layer was dried with magnesium sulfate and filtered. The filtrate was concentrated under reduced pressure to a residual oil. The oil was distilled under vacuum, yielding about 9.0 grams of 3-(4-chlorophenoxy)phenyl bromide, bp 110° C./0.5 mm Hg. The NMR spectrum was consistent with the proposed structure.

후처리

  1. additionUpon completion of addition
  2. customto remove methanol
  3. customAfter the methanol was removed
  4. temperatureUpon completion of the additions, the reaction mixture was heated
  5. temperatureto reflux where it
  6. temperatureThe reaction mixture was then cooled
  7. filtrationfiltered
  8. washThe filter cake was washed with diethyl ether
  9. extractionThe combination was extracted with two 20 mL portions of aqueous 20% sodium hydroxide
  10. dry with materialThe organic layer was dried with magnesium sulfate
  11. filtrationfiltered
  12. concentrationThe filtrate was concentrated under reduced pressure to a residual oil
  13. distillationThe oil was distilled under vacuum

출처 및 근거

ORD 기록
ord-e9bd9eca68c34efda2b6be9b01191344
출처 데이터셋
uspto-grants-1997_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05616718

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