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Hydrochloric Acid → 5-(4-bromo-2-formyl-N-propylanilino)pentanoic acid

HRID 402258
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HRID 402258 반응식
[CH2:1]([N:4]1C[CH2:8][CH2:7][CH2:6][C:5]1=O)[CH2:2][CH3:3].[OH-].[Na+].Cl.[C:14](=[O:17])([O-])[O-:15].[Na+].[Na+].[Br:20][C:21]1[CH:22]=[CH:23][C:24](F)=[C:25]([CH:28]=1)[CH:26]=[O:27]>O.CS(C)=O>[Br:20][C:21]1[CH:22]=[CH:23][C:24]([N:4]([CH2:5][CH2:6][CH2:7][CH2:8][C:14]([OH:15])=[O:17])[CH2:1][CH2:2][CH3:3])=[C:25]([CH:26]=[O:27])[CH:28]=1
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참가 물질

8

반응물 5

HCID 313Hydrochloric AcidHCID 10340Sodium CarbonateHCID 14798Sodium HydroxideHCID 7363275-Bromo-2-fluorobenzaldehydeHCID 109425321-Propylpiperidin-2-one

생성물 1

HCID 865955795-(4-bromo-2-formyl-N-propylanilino)pentanoic acid수율 96.7%

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 962Water용매

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온도
0 °C

실험 절차

A mixture of 1-propyl-2-piperidone (7.5 g) and 4N sodium hydroxide (26.6 ml) was refluxed for 4 hours. The mixture was cooled to 0° C. and conc. hydrochloric acid (8.85 ml) was added thereto. To the mixture were added sodium carbonate (11.3 g), 5-bromo-2-fluorobenzaldehyde (5.4 g) and DMSO (70 ml), and the resulting mixture was heated at 135° C. for 6 hours. The mixture was allowed to cool. Water was added and the mixture was extracted with THF-ethyl acetate. The organic layer was washed with water and saturated saline, and dried over magnesium sulfate. After distilling off the solvent under reduced pressure, the residue was purified by silica gel column chromatography to obtain brown oil of 5-(4-bromo-2-formyl-N-propylanilino)pentanoic acid (8.8 g)

후처리

  1. temperaturewas refluxed for 4 hours
  2. temperaturethe resulting mixture was heated at 135° C. for 6 hours
  3. temperatureto cool
  4. extractionthe mixture was extracted with THF-ethyl acetate
  5. washThe organic layer was washed with water and saturated saline
  6. dry with materialdried over magnesium sulfate
  7. distillationAfter distilling off the solvent under reduced pressure
  8. customthe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-44c23033537547e6a4a2f611cde06f15
출처 데이터셋
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08741943B2

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