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2,6-Lutidine → HCID 178438536, 화합물

HRID 1688992
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HRID 1688992 반응식
[F:1][C:2]1[CH:3]=[C:4]([C:29]2[C:30]([C:35]#[N:36])=[CH:31][CH:32]=[CH:33][CH:34]=2)[CH:5]=[CH:6][C:7]=1[CH2:8][C:9]1[C:10](=[O:28])[N:11]([C@H:21]2[CH2:26][CH2:25][C@@H:24]([OH:27])[CH2:23][CH2:22]2)[C:12]2[N:13]([N:18]=[CH:19][N:20]=2)[C:14]=1[CH2:15][CH2:16][CH3:17].FC(F)(F)S(O[Si](C(C)(C)C)(C)C)(=O)=O.[N:52]1C(C)=CC=CC=1C.[Cl-].O[NH3+].[C:63](=[O:66])([O-])[OH:64].[Na+]>C(OCC)(=O)C.CS(C)=O.O1CCCC1>[F:1][C:2]1[CH:3]=[C:4]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][C:30]=2[C:35]2[NH:52][C:63](=[O:66])[O:64][N:36]=2)[CH:5]=[CH:6][C:7]=1[CH2:8][C:9]1[C:10](=[O:28])[N:11]([C@H:21]2[CH2:26][CH2:25][C@@H:24]([OH:27])[CH2:23][CH2:22]2)[C:12]2[N:13]([N:18]=[CH:19][N:20]=2)[C:14]=1[CH2:15][CH2:16][CH3:17]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 5

HCID 79372,6-LutidineHCID 21645Hydroxylamine HClHCID 123564tert-Butyldimethylsilyl trifluoromethanesulphonateHCID 516892Sodium BicarbonateHCID 178438708HCID 178438708, 화합물

생성물 1

HCID 178438536HCID 178438536, 화합물수율 38%

시약·촉매·용매 3

HCID 679Dimethyl Sulfoxide용매2회HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매2회

반응 조건

온도
0 °C

실험 절차

A mixture of 3′-fluoro-4′-{[4-(cis-4-hydroxycyclohexyl)-5-oxo-7-propyl-4,5-dihydro[1,2,4]triazolo[1,5-a]pyrimidin-6-yl]methyl}biphenyl-2-carbonitrile (0.085 g), tert-butyl(dimethyl)silyl trifluoromethanesulfonate (0.06 mL), 2,6-lutidine (0.03 mL) and tetrahydrofuran (5 mL) was stirred at 0° C. for 3 hr. The reaction mixture was diluted with ethyl acetate, washed with water and then with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The residue obtained by silica gel column chromatography was dissolved in dimethyl sulfoxide (5 mL), and the mixture was added to a mixture of hydroxylammonium chloride (0.18 g), sodium hydrogen carbonate (0.29 g) and dimethyl sulfoxide (5 mL), which had been stirred in advance at 40° C. for 30 min. The reaction mixture was stirred at 90° C. for 16 hr, diluted with ethyl acetate, washed with water and then with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was dissolved in tetrahydrofuran (5 mL). N,N′-Carbonyldiimidazole (0.034 g) and then 1,8-diazabicyclo[5.4.0]undec-7-ene (0.029 mL) were added, and the mixture was stirred at room temperature for 2 hr. The reaction mixture was diluted with ethyl acetate, washed with saturated aqueous potassium hydrogensulfate solution and then with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was dissolved in tetrahydrofuran (10 mL). Tetrabutylammonium bromide (1.0 M tetrahydrofuran solution, 0.44 mL) was added, and the mixture was stirred at room temperature for 3 hr. The reaction mixture was extracted with 1 N hydrochloric acid and ethyl acetate, and the ethyl acetate layer was washed with saturated brine and concentrated. The residue was purified by silica gel column chromatography to give the title compound as a colorless amorphous solid (0.036 g, 38%).

후처리

  1. washwashed with water
  2. dry with materialwith saturated brine, and dried over anhydrous magnesium sulfate
  3. customThe solvent was evaporated under reduced pressure
  4. customThe residue obtained by silica gel column chromatography
  5. stirringhad been stirred in advance at 40° C. for 30 min
  6. stirringThe reaction mixture was stirred at 90° C. for 16 hr
  7. washwashed with water
  8. dry with materialwith saturated brine, and dried over anhydrous magnesium sulfate
  9. customThe solvent was evaporated under reduced pressure
  10. dissolutionthe residue was dissolved in tetrahydrofuran (5 mL)
  11. additionN,N′-Carbonyldiimidazole (0.034 g) and then 1,8-diazabicyclo[5.4.0]undec-7-ene (0.029 mL) were added
  12. stirringthe mixture was stirred at room temperature for 2 hr
  13. additionThe reaction mixture was diluted with ethyl acetate
  14. washwashed with saturated aqueous potassium hydrogensulfate solution
  15. dry with materialwith saturated brine, and dried over anhydrous magnesium sulfate
  16. customThe solvent was evaporated under reduced pressure
  17. dissolutionthe residue was dissolved in tetrahydrofuran (10 mL)
  18. additionTetrabutylammonium bromide (1.0 M tetrahydrofuran solution, 0.44 mL) was added
  19. stirringthe mixture was stirred at room temperature for 3 hr
  20. extractionThe reaction mixture was extracted with 1 N hydrochloric acid and ethyl acetate
  21. washthe ethyl acetate layer was washed with saturated brine
  22. concentrationconcentrated
  23. customThe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-4e5027c0a3934efaaf2c32c989a49ac9
출처 데이터셋
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08148383B2

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