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3-Bromobenzaldehyde → 1-Bromo-3-(2-methyl-1-propenyl)benzene

HRID 1594944
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HRID 1594944 반응식
[I-].[CH:2]([P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)([CH3:4])[CH3:3].C([Li])CCC.[Br:29][C:30]1[CH:31]=[C:32]([CH:35]=[CH:36][CH:37]=1)[CH:33]=O>C1COCC1>[CH:33]([C:32]1[CH:31]=[C:30]([Br:29])[CH:37]=[CH:36][CH:35]=1)=[C:2]([CH3:4])[CH3:3]
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참가 물질

5

반응물 3

HCID 765833-BromobenzaldehydeHCID 2723783Isopropyltriphenylphosphonium iodideHCID 178418339Butyllithium

생성물 1

HCID 217068361-Bromo-3-(2-methyl-1-propenyl)benzene수율 79%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
-23 °C

실험 절차

To a suspension of iso-propyltriphenylphosphonium iodide in dry THF (150 mL) under nitrogen at −23° C. was added 2.5 M n-butyl lithium in hexanes (13.4 mL, 33.6 mmol). The resulting solution was stirred 0.5 hours at −23° C., the cooling bath was removed, and the reaction was stirred 0.5 hours at ambient temperature to give a dark red homogeneous solution which was cooled to −23° C. To the solution was added neat 3-bromobenzaldehyde (3.73 mL, 32 mmol). The cooling bath was removed, the reaction was stirred at ambient temperature for 1 hour, quenched by adding excess saturated ammonium chloride, and partitioned between ether and brine. The organic layer was washed with saturated aqueous Na2S2O5, brine, dried (Na2SO4), filtered, and concentrated under vacuum. Purification on silica gel with hexanes gave the title compound (5.34 g, 79%) as a colorless oil.

후처리

  1. customthe cooling bath was removed
  2. stirringthe reaction was stirred 0.5 hours at ambient temperature
  3. customto give a dark red homogeneous solution which
  4. temperaturewas cooled to −23° C
  5. customThe cooling bath was removed
  6. stirringthe reaction was stirred at ambient temperature for 1 hour
  7. customquenched
  8. additionby adding excess saturated ammonium chloride
  9. custompartitioned between ether and brine
  10. washThe organic layer was washed with saturated aqueous Na2S2O5, brine
  11. dry with materialdried (Na2SO4)
  12. filtrationfiltered
  13. concentrationconcentrated under vacuum
  14. customPurification on silica gel with hexanes

출처 및 근거

ORD 기록
ord-156aa50acb8d4a6ab5bdfdd0c739052b
출처 데이터셋
uspto-grants-2001_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06284796B1

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