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Hexane → 6-((2S)-2-(1-(3-chloropyridin-2-yl)-1H-pyrazolo[3,4-d]pyrimidin-4-yloxy)-3-isopropoxypropanamido)-N,N-dimethylnicotinamide

HRID 1098031
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HRID 1098031 반응식
C[Al](C)C.[NH2:5][C:6]1[CH:16]=[CH:15][C:9]([C:10]([N:12]([CH3:14])[CH3:13])=[O:11])=[CH:8][N:7]=1.[Cl:17][C:18]1[C:19]([N:24]2[C:28]3=[N:29][CH:30]=[N:31][C:32]([O:33][C@@H:34]([CH2:39][O:40][CH:41]([CH3:43])[CH3:42])[C:35](OC)=[O:36])=[C:27]3[CH:26]=[N:25]2)=[N:20][CH:21]=[CH:22][CH:23]=1.CCCCCC>C1(C)C=CC=CC=1>[Cl:17][C:18]1[C:19]([N:24]2[C:28]3=[N:29][CH:30]=[N:31][C:32]([O:33][C@@H:34]([CH2:39][O:40][CH:41]([CH3:43])[CH3:42])[C:35]([NH:5][C:6]4[CH:16]=[CH:15][C:9]([C:10]([N:12]([CH3:14])[CH3:13])=[O:11])=[CH:8][N:7]=4)=[O:36])=[C:27]3[CH:26]=[N:25]2)=[N:20][CH:21]=[CH:22][CH:23]=1
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참가 물질

6

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HCID 8058HexaneHCID 16682925Trimethylaluminum2회HCID 575045326-amino-N,N-dimethylpyridine-3-carboxamide2회HCID 59279531(2S)-Methyl 2-(1-(3-chloropyridin-2-yl)-1H-pyrazolo[3,4-d]pyrimidin-4-yloxy)-3-isopropoxypropanoate

생성물 1

HCID 575044086-((2S)-2-(1-(3-chloropyridin-2-yl)-1H-pyrazolo[3,4-d]pyrimidin-4-yloxy)-3-isopropoxypropanamido)-N,N-dimethylnicotinamide

시약·촉매·용매 1

HCID 1140Toluene용매3회

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온도
0 °C

실험 절차

Trimethylaluminium (2M in hexane, 0.376 mL, 0.75 mmol) was added to 6-amino-N,N-dimethylnicotinamide (CAS no. 827588-33-0) (108 mg, 0.65 mmol) in toluene (20 mL) at 0° C. under Nitrogen. The resulting solution was stirred at 0° C. for 20 minutes. (2S)-Methyl 2-(1-(3-chloropyridin-2-yl)-1H-pyrazolo[3,4-d]pyrimidin-4-yloxy)-3-isopropoxypropanoate (Intermediate L1) (256 mg, 0.65 mmol) in toluene (6 mL) was added dropwise at this temperature. After the addition was complete, the solution was allowed to warm to ambient temperature and was then heated to reflux for 16 hours. Allowed to cool to ambient temperature. The reaction mixture was concentrated and diluted with EtOAc (100 mL) and washed with saturated brine (50 mL). The organic layer was dried (MgSO4), filtered and evaporated. 2M Trimethylaluminium in hexane (0.376 mL, 0.75 mmol) was added to 6-amino-N,N-dimethylnicotinamide (108 mg, 0.65 mmol) in toluene (20 mL) at 0° C. under Nitrogen. The resulting solution was stirred at 0° C. for 20 minutes. The residue from the above evaporation was dissolved in toluene (6 mL) and added dropwise. After the addition was complete, the solution was allowed to warm to ambient temperature and was then heated to reflux for 16 hours. Allowed to cool to ambient temperature. The reaction mixture was concentrated and diluted with EtOAc (100 mL) and washed with saturated brine (50 mL). The organic layer was dried (MgSO4), filtered and evaporated to afford crude product.

후처리

  1. customat 0° C.
  2. additionAfter the addition
  3. temperatureto warm to ambient temperature
  4. temperaturewas then heated
  5. temperatureto reflux for 16 hours
  6. temperatureAllowed to cool to ambient temperature
  7. concentrationThe reaction mixture was concentrated
  8. additiondiluted with EtOAc (100 mL)
  9. washwashed with saturated brine (50 mL)
  10. dry with materialThe organic layer was dried (MgSO4)
  11. filtrationfiltered
  12. customevaporated
  13. stirringThe resulting solution was stirred at 0° C. for 20 minutes
  14. customThe residue from the above evaporation
  15. dissolutionwas dissolved in toluene (6 mL)
  16. additionadded dropwise
  17. additionAfter the addition
  18. temperatureto warm to ambient temperature
  19. temperaturewas then heated
  20. temperatureto reflux for 16 hours
  21. temperatureAllowed to cool to ambient temperature
  22. concentrationThe reaction mixture was concentrated
  23. additiondiluted with EtOAc (100 mL)
  24. washwashed with saturated brine (50 mL)
  25. dry with materialThe organic layer was dried (MgSO4)
  26. filtrationfiltered
  27. customevaporated
  28. customto afford crude product

출처 및 근거

ORD 기록
ord-ccc42f852965467db8ffc6d8d7faa1bb
출처 데이터셋
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08143263B2

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