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Triethylamine → 3-(4-Phenyl-3,6-dihydropyridin-1(2H)-yl)propanoic acid

HRID 239721
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HRID 239721 반응식
Cl.[C:2]1([C:8]2[CH2:9][CH2:10][NH:11][CH2:12][CH:13]=2)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(N(CC)CC)C.Br[CH2:22][CH2:23][C:24]([O:26]C)=[O:25]>C(Cl)Cl>[C:2]1([C:8]2[CH2:13][CH2:12][N:11]([CH2:22][CH2:23][C:24]([OH:26])=[O:25])[CH2:10][CH:9]=2)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 76934Methyl 3-bromopropanoateHCID 27238604-Phenyl-1,2,3,6-tetrahydropyridine hydrochloride

생성물 1

HCID 597714703-(4-Phenyl-3,6-dihydropyridin-1(2H)-yl)propanoic acid

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

The 4-phenyl-1,2,3,6-tetrahydropyridine hydrochloride (1.5 g, 7.8 mmol) suspended in 16 mL of CH2Cl2. To this suspension was added triethylamine (2.1 mL, 15.3 mmol) followed by methyl 3-bromopropionate (1.0 mL, 9.2 mmol). The reaction was stirred at room temperature for 4 h and at reflux for 2 h. The reaction mixture was washed with water, 1N HCl (2×20 mL), 1N NaOH (2×20 mL) and Brine (1×20 mL). The organic layer was separated, dried over Na2SO4, filtered; and solvent was removed under reduced pressure. To the crude product was added 2N NaOH (15 mL). The mixture was stirred at reflux for 1 h. The reaction mixture was washed with CH2Cl2 (3×20 mL) and neutralized with concentrated HCl. The aqueous solution was concentrated to dryness under reduced pressure, to give a solid residue. Sodium chloride in the residue was removed in the following way (three repeats): dissolving the residue in a minimum amount of water, treating the aqueous solution with acetone, removing the resultant solid material by filtration, and concentrate the filtrate to dryness under reduced pressure. This allowed the isolation of compound Q (159.4 mg).

후처리

  1. temperatureat reflux for 2 h
  2. washThe reaction mixture was washed with water, 1N HCl (2×20 mL), 1N NaOH (2×20 mL) and Brine (1×20 mL)
  3. customThe organic layer was separated
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. customand solvent was removed under reduced pressure
  7. additionTo the crude product was added 2N NaOH (15 mL)
  8. stirringThe mixture was stirred
  9. temperatureat reflux for 1 h
  10. washThe reaction mixture was washed with CH2Cl2 (3×20 mL) and neutralized with concentrated HCl
  11. concentrationThe aqueous solution was concentrated to dryness under reduced pressure
  12. customto give a solid residue
  13. customSodium chloride in the residue was removed in the following way (three repeats)
  14. dissolutiondissolving the residue in a minimum amount of water
  15. additiontreating the aqueous solution with acetone
  16. customremoving the resultant solid material
  17. filtrationby filtration
  18. concentrationconcentrate the filtrate to dryness under reduced pressure

출처 및 근거

ORD 기록
ord-7b74e9a64ffa4bd8ad0b8ad77561e551
출처 데이터셋
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08642801B2

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