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Imidazole → (4R)-2-(3-(tert-butyldimethylsilyloxy)benzyl)-4-(tetrahydro-2H-pyran-2-yloxy)cyclopent-2-e none

HRID 1803642
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HRID 1803642 반응식
C([O:8][C:9]1[CH:10]=[C:11]([CH:20]=[CH:21][CH:22]=1)[CH2:12][C:13]1[C:14](=[O:19])[CH2:15][C@@H:16]([OH:18])[CH:17]=1)C1C=CC=CC=1.[O:23]1[CH:28]=[CH:27][CH2:26][CH2:25][CH2:24]1.C1(C)C=CC(S(O)(=O)=O)=CC=1.N1C=CN=C1.[Si:45](Cl)([C:48]([CH3:51])([CH3:50])[CH3:49])([CH3:47])[CH3:46]>C(Cl)Cl>[Si:45]([O:8][C:9]1[CH:10]=[C:11]([CH:20]=[CH:21][CH:22]=1)[CH2:12][C:13]1[C:14](=[O:19])[CH2:15][C@@H:16]([O:18][CH:28]2[CH2:27][CH2:26][CH2:25][CH2:24][O:23]2)[CH:17]=1)([C:48]([CH3:51])([CH3:50])[CH3:49])([CH3:47])[CH3:46]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 795ImidazoleHCID 6101p-Toluenesulfonic acidHCID 80803,4-dihydro-2H-pyranHCID 28928tert-Butyldimethylsilyl chlorideHCID 71170047(R)-4-hydroxy-2-(3-benzyloxybenzyl)cyclopent-2-enone

생성물 1

HCID 71270576(4R)-2-(3-(tert-butyldimethylsilyloxy)benzyl)-4-(tetrahydro-2H-pyran-2-yloxy)cyclopent-2-e none
수율 69%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

(R)-2-(3-(benzyloxy)benzyl)-4-hydroxycyclopent-2-enone (0.5 g, 1.7 mmol) and dihydropyrane (0.34 g, 4 mmol) was dissolved in CH2Cl2 (5 ml), p-toluenesulfonic acid (0.2 g) was added to the solution at 10° C., and the mixture was stirred at room temperature overnight. After the reaction was completed, the mixture was washed with sat. NaHCO3 aq., dried over MgSO4, and evaporated. The resulting residue was dissolved in EtOH (5 ml) under hydrogen, Pd/C (0.15 g) was added to the solution and the mixture was stirred at room temperature for 2 hrs. After the reaction was completed, the reaction mixture was filtered to remove the Pd/C and the filtrate was evaporated. The resulting residue was dissolved in EtOAc (5 ml), imidazole (0.24 g, 3.5 mmol) and tert-butyldimethylsilyl chloride (0.38 g, 2.55 mmol) was added to the solution and the mixture was stirred at 50° C. for 4 hrs. After the reaction was completed, the reaction mixture was filtered to remove the precipitate and washed with NaHCO3 and extracted with EtOAc. The organic layer was dried over MgSO4, and evaporated. The residue was purified by chromatography on a silica gel column using hexane-EtOAc as eluent to give (4R)-2-(3-(tert-butyldimethylsilyloxy)benzyl)-4-(tetrahydro-2H-pyran-2-yloxy)cyclopent-2-e none as yellow oil: 0.47 g (yield: 69%,)

후처리

  1. washthe mixture was washed with sat. NaHCO3 aq.
  2. dry with materialdried over MgSO4
  3. customevaporated
  4. dissolutionThe resulting residue was dissolved in EtOH (5 ml) under hydrogen
  5. additionPd/C (0.15 g) was added to the solution
  6. stirringthe mixture was stirred at room temperature for 2 hrs
  7. filtrationthe reaction mixture was filtered
  8. customto remove the Pd/C
  9. customthe filtrate was evaporated
  10. dissolutionThe resulting residue was dissolved in EtOAc (5 ml)
  11. stirringthe mixture was stirred at 50° C. for 4 hrs
  12. filtrationthe reaction mixture was filtered
  13. customto remove the precipitate
  14. washwashed with NaHCO3
  15. extractionextracted with EtOAc
  16. dry with materialThe organic layer was dried over MgSO4
  17. customevaporated
  18. customThe residue was purified by chromatography on a silica gel column

출처 및 근거

ORD 기록
ord-6d42f016cd99487babd27b167bb9e9f9
출처 데이터셋
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08350090B1

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