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3-Hydroxybenzaldehyde → HCID 44538142, 화합물

HRID 1015678
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HRID 1015678 반응식
[OH:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH:5]=O.Br[CH2:11][CH2:12][CH2:13][CH2:14][Cl:15].C(=O)([O-])[O-].[K+].[K+].[BH4-].[Na+].[CH3:24][O:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=1[N:32]1[CH2:37][CH2:36][NH:35][CH2:34][CH2:33]1.C(=O)([O-])[O-].[Na+].[Na+].[I-].[K+].S(Cl)(Cl)=O.[NH:50]1[CH:54]=[CH:53][N:52]=[CH:51]1>CC(C)=O.O.N1C=CC=CC=1>[ClH:15].[N:50]1([CH2:5][C:4]2[CH:3]=[C:2]([CH:9]=[CH:8][CH:7]=2)[O:1][CH2:11][CH2:12][CH2:13][CH2:14][N:35]2[CH2:36][CH2:37][N:32]([C:27]3[CH:28]=[CH:29][CH:30]=[CH:31][C:26]=3[O:25][CH3:24])[CH2:33][CH2:34]2)[CH:54]=[CH:53][N:52]=[CH:51]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

13

반응물 9

HCID 1013-HydroxybenzaldehydeHCID 795ImidazoleHCID 13461-(2-Methoxyphenyl)piperazineHCID 4875Potassium Iodide2회HCID 10340Sodium CarbonateHCID 11430Potassium Carbonate2회HCID 24386Thionyl Chloride
HCID 81364
1-Bromo-4-chlorobutane
HCID 4311764Sodium borohydride

생성물 1

HCID 44538142HCID 44538142, 화합물

시약·촉매·용매 3

HCID 180Acetone용매HCID 962Water용매HCID 1049Pyridine용매

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온도
25 °C

실험 절차

A mixture of 3-hydroxybenzaldehyde (5 mmol), 1-bromo-4-chlorobutane (5 mmol), and potassium carbonate (15 mmol) was refluxed in 100 ml of acetone for 6 h. This solution was then concentrated in a rotary evaporator and diluted with ethyl acetate, then washed with brine, and the resulting organic layer was dried and purified by column chromatography. This was dissolved in methanol (50 ml) and was added with sodium borohydride (10 mmol) at 25° C., and was stirred at 25° C. for 2 h. This solution was then concentrated in a rotary evaporator and diluted with methylene chloride, then washed with brine, and the resulting organic layer was dried and concentrated in vacuo. The crude product was dissolved in isopropanol (50 ml) and was added with 1-(2-methoxyphenyl)-piperazine (5 mmol), sodium carbonate (15 mmol), and potassium iodide (5 mmol) at 25° C., and the reaction mixture was refluxed for 12 h. This solution was then concentrated in a rotary evaporator and diluted with methylene chloride, then washed with brine, and the resulting organic layer was dried and purified by column chromatography. This product was dissolved in CHCl3 (30 ml) and was added with pyridine and thionyl chloride (5 mmol) at 0° C., and then the resulting reaction mixture was stirred at room temperature for 16 h, and water was added to terminate the reaction. The organic layer was extracted 3 times with dichloromethane, then dried and concentrated in vacuo, and the residue was purified by column chromatography. This was dissolved in acetonitrile (30 ml) and was added with imidazole (6 mmol), potassium carbonate (15 mmol), and potassium iodide (5 mmol) at 25° C., and the reaction mixture was refluxed for 12 h. This solution was then concentrated in a rotary evaporator and diluted with methylene chloride, then washed with brine, and the resulting organic layer was dried and purified by column chromatography. The resulting 1-[4-(3-imidazole-1-ylmethyl-phenoxy)-butyl]-4-(2-methoxy-phenyl)-piperazine was dissolved in dichloromethane and the solution was treated with a solution of HCl in ethyl ether. The resulting precipitate was filtered to give 1-[4-(3-imidazol-1-ylmethyl-phenoxy)-butyl]-4-(2-methoxy-phenyl)-piperazine hydrochloride.

후처리

  1. concentrationThis solution was then concentrated in a rotary evaporator
  2. additiondiluted with ethyl acetate
  3. washwashed with brine
  4. customthe resulting organic layer was dried
  5. custompurified by column chromatography
  6. dissolutionThis was dissolved in methanol (50 ml)
  7. concentrationThis solution was then concentrated in a rotary evaporator
  8. additiondiluted with methylene chloride
  9. washwashed with brine
  10. customthe resulting organic layer was dried
  11. concentrationconcentrated in vacuo
  12. dissolutionThe crude product was dissolved in isopropanol (50 ml)
  13. temperaturethe reaction mixture was refluxed for 12 h
  14. concentrationThis solution was then concentrated in a rotary evaporator
  15. additiondiluted with methylene chloride
  16. washwashed with brine
  17. customthe resulting organic layer was dried
  18. custompurified by column chromatography
  19. dissolutionThis product was dissolved in CHCl3 (30 ml)
  20. customthe resulting reaction mixture
  21. stirringwas stirred at room temperature for 16 h
  22. customto terminate
  23. customthe reaction
  24. extractionThe organic layer was extracted 3 times with dichloromethane
  25. customdried
  26. concentrationconcentrated in vacuo
  27. customthe residue was purified by column chromatography
  28. dissolutionThis was dissolved in acetonitrile (30 ml)
  29. temperaturethe reaction mixture was refluxed for 12 h
  30. concentrationThis solution was then concentrated in a rotary evaporator
  31. additiondiluted with methylene chloride
  32. washwashed with brine
  33. customthe resulting organic layer was dried
  34. custompurified by column chromatography
  35. dissolutionThe resulting 1-[4-(3-imidazole-1-ylmethyl-phenoxy)-butyl]-4-(2-methoxy-phenyl)-piperazine was dissolved in dichloromethane
  36. additionthe solution was treated with a solution of HCl in ethyl ether
  37. filtrationThe resulting precipitate was filtered

출처 및 근거

ORD 기록
ord-ac3d0defcd4943d2b28779fabaf50124
출처 데이터셋
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07985752B2

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