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Hydrochloric Acid → 3-(4-Bromophenyl)piperidine

HRID 1784707
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HRID 1784707 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]2[CH2:13][CH2:12][CH2:11][NH:10][C:9]2=O)=[CH:4][CH:3]=1.B.O1CCCC1.Cl>O1CCCC1>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([CH:8]2[CH2:13][CH2:12][CH2:11][NH:10][CH2:9]2)=[CH:6][CH:7]=1
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참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 2723981Borane;tetrahydrofuranHCID 468400403-(4-Bromophenyl)piperidin-2-one

생성물 1

HCID 468353263-(4-Bromophenyl)piperidine수율 90%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To an ice-cooled solution of 3-(4-bromo-phenyl)-piperidin-2-one (37.97 g, 149 mmol) in tetrahydrofuran (250 ml) was added borane-tetrahydrofuran complex (335 ml, 1.0 M solution in THF, 335 mmol). The solution was stirred overnight at room temperature, and then refluxed 1.5 hr after addition of 10% aqueous hydrochloric acid. Solvents was removed in vacuo, and the residue was partitioned between dichloromethane and 1N sodium hydroxide. The aqueous layer was extracted with dichlorometane. The combined organic layer was washed with water and brine, dried over sodium sulfate, and concentrated in vacuo. The residue was dissolved in water (100 mL) and concentrated hydrochloric acid (100 mL) and refluxed for 3 hr. Sodium hydroxide was added to the solution and the resulting solution was extracted with dichlorometane. The organic layer was washed with water and brine, dried over sodium sulfate Concentration in vacuo afforded 3-(4-bromo-phenyl)-piperidine (32 18 g, 90%).

후처리

  1. temperaturerefluxed 1.5 hr
  2. customSolvents was removed in vacuo
  3. customthe residue was partitioned between dichloromethane and 1N sodium hydroxide
  4. extractionThe aqueous layer was extracted with dichlorometane
  5. washThe combined organic layer was washed with water and brine
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated in vacuo
  8. dissolutionThe residue was dissolved in water (100 mL)
  9. temperatureconcentrated hydrochloric acid (100 mL) and refluxed for 3 hr
  10. additionSodium hydroxide was added to the solution
  11. extractionthe resulting solution was extracted with dichlorometane
  12. washThe organic layer was washed with water and brine
  13. dry with materialdried over sodium sulfate Concentration in vacuo

출처 및 근거

ORD 기록
ord-6d4e95c7133d42b48eeb2ffe5e987cab
출처 데이터셋
uspto-grants-2009_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07504411B2

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