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Dimethyl Sulfoxide → 4-(5-(1-(pyridin-2-yl)-5-(trifluoromethyl)-1H-pyrazol-4-yl)-1,2,4-oxadiazol-3-yl)benzaldehyde

HRID 1941885
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HRID 1941885 반응식
C(Cl)(=O)C(Cl)=O.CS(C)=O.[N:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[N:17]1[C:21]([C:22]([F:25])([F:24])[F:23])=[C:20]([C:26]2[O:30][N:29]=[C:28]([C:31]3[CH:36]=[CH:35][C:34]([CH2:37][OH:38])=[CH:33][CH:32]=3)[N:27]=2)[CH:19]=[N:18]1.CCN(C(C)C)C(C)C>C(Cl)Cl>[N:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[N:17]1[C:21]([C:22]([F:23])([F:24])[F:25])=[C:20]([C:26]2[O:30][N:29]=[C:28]([C:31]3[CH:32]=[CH:33][C:34]([CH:37]=[O:38])=[CH:35][CH:36]=3)[N:27]=2)[CH:19]=[N:18]1
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참가 물질

6

반응물 4

HCID 679Dimethyl SulfoxideHCID 65578Oxalyl chlorideHCID 81531DiisopropylethylamineHCID 66996907(4-(5-(1-(pyridin-2-yl)-5-(trifluoromethyl)-1H-pyrazol-4-yl)-1,2,4-oxadiazol-3-yl)phenyl)methanol

생성물 1

HCID 866590394-(5-(1-(pyridin-2-yl)-5-(trifluoromethyl)-1H-pyrazol-4-yl)-1,2,4-oxadiazol-3-yl)benzaldehyde수율 67.4%

시약·촉매·용매

1
HCID 6344Dichloromethane용매2회

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온도
-78 °C

실험 절차

300 mL of DCM was cooled to −78° C., then oxalyl chloride (0.475 mL, 5.42 mmol) was added and the mixture was stirred at −78° C. for 10 min. DMSO (0.586 mL, 8.26 mmol) was added and the mixture was stirred at −78° C. for 15 min. A solution of (4-(5-(1-(pyridin-2-yl)-5-(trifluoromethyl)-1H-pyrazol-4-yl)-1,2,4-oxadiazol-3-yl)phenyl)methanol (1 g, 2.58 mmol) in 60 mL of DCM was added dropwise over 10 minutes into the reaction mixture, with the SM flask being rinsed with another 10 mL of DCM which was also added into the reaction dropwise. The reaction was kept at −78° C. for 40 min, then Hunig's Base (3.61 mL, 20.66 mmol) was added over 10 minutes. Stirring at −78° C. continued for 10 min, then the dry ice bath was removed and the reaction flask gradually warmed to room temperature. A 0.5 N KHSO4 solution (70 mL) was added and the mixture was extracted twice with DCM (50 mL). The organics were combined, dried with Na2SO4, and concentrated. Diethyl ether (100 mL) was added to the product, with the mixture being stirred overnight, then filtered and the solids washed with diethyl ether to afford 4-(5-(1-(pyridin-2-yl)-5-(trifluoromethyl)-1H-pyrazol-4-yl)-1,2,4-oxadiazol-3-yl)benzaldehyde (700 mg, 1.74 mmol). The compound had an HPLC retention time=3.69 min.−Column: CHROMOLITH® SpeedROD 4.6×50 mm (4 min.); Solvent A=10% MeOH, 90% H2O, 0.2% H3PO4; Solvent B=90% MeOH, 10% H2O, 0.2% H3PO4. LC/MS M+1=386.01. 1H NMR (400 MHz, DMSO-d6) δ ppm 7.69 (ddd, J=0.8 Hz, 5.0 Hz, 7.4 Hz, 1H), 7.90 (d, J=8.0 Hz, 1H), 8.15 (d, J=8.3 Hz, 2H), 8.20 (dt, J=1.9 Hz, 7.7 Hz, 1H), 8.32 (d, J=8.3 Hz, 2H), 8.67 (dd, J=1.9 Hz, 4.7 Hz, 1H), 8.76 (s, 1H), 10.13 (s, 1H)

후처리

  1. stirringthe mixture was stirred at −78° C. for 15 min
  2. washbeing rinsed with another 10 mL of DCM which
  3. additionwas also added into the reaction dropwise
  4. waitThe reaction was kept at −78° C. for 40 min
  5. stirringStirring at −78° C.
  6. waitcontinued for 10 min
  7. customthe dry ice bath was removed
  8. temperaturethe reaction flask gradually warmed to room temperature
  9. additionA 0.5 N KHSO4 solution (70 mL) was added
  10. extractionthe mixture was extracted twice with DCM (50 mL)
  11. dry with materialdried with Na2SO4
  12. concentrationconcentrated
  13. additionDiethyl ether (100 mL) was added to the product, with the mixture
  14. stirringbeing stirred overnight
  15. filtrationfiltered
  16. washthe solids washed with diethyl ether

출처 및 근거

ORD 기록
ord-fcb9849d08ac44b592ff869c99790169
출처 데이터셋
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08389509B2

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