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Methanol → HCID 58072381, Verbindung

HRID 2089956
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2089956
[C:1]([C:5]1[C:10](=[O:11])[CH:9]=[CH:8][N:7]([C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([C:18]([F:21])([F:20])[F:19])[CH:13]=2)[N:6]=1)(=O)[CH2:2][CH3:3].[CH3:22][O-].[Na+].[C:25]1([NH:31][NH2:32])[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1.CO>C(OC)=O.O.Cl>[CH3:3][C:2]1[CH:22]=[N:32][N:31]([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[C:1]=1[C:5]1[C:10](=[O:11])[CH:9]=[CH:8][N:7]([C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([C:18]([F:21])([F:20])[F:19])[CH:13]=2)[N:6]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 4

HCID 887MethanolHCID 7516PhenylhydrazineHCID 10942334Sodium MethoxideHCID 58072182HCID 58072182, Verbindung

Produkt 1

HCID 58072381HCID 58072381, VerbindungAusbeute 39 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 313
Hydrochloric Acid
Lösungsmittel
2×
HCID 962WaterLösungsmittel
HCID 7865Methyl formateLösungsmittel

Versuchsvorschrift

To a suspension of 3-propanoyl-1-[3-(trifluoromethyl)phenyl]pyridazin-4(1H)-one (384 mg, 1.30 mmol) in methyl formate (3.8 mL) was added NaOMe (28% in MeOH, 326 mg, 1.69 mmol) at room temperature. The mixture was stirred at room temperature for 3.5 h. The mixture was diluted with water and 1 M HCl aqueous solution, extracted with AcOEt, washed with brine, dried over Na2SO4, filtered, concentrated in vacuo and crystallized with AcOEt/hexane. To the solid were added phenylhydrazine (0.405 mL, 4.12 mmol) and MeOH (6.7 mL). The mixture was heated to reflux for 15 h. The mixture was diluted with 1 M HCl aqueous solution, extracted with AcOEt, washed with saturated NaHCO3 aqueous solution, dried over Na2SO4, filtered, concentrated in vacuo, purified by column chromatography on silica gel (hexane/AcOEt=50/50 to 0/100) and crystallized with AcOEt/heptane to yield the title compound (161 mg, 39% yield) as a pale yellow solid: mp 208-211° C. 1H NMR (DMSO-d6, 300 MHz): δ ppm 2.09 (3H, s), 6.62 (1H, d, J=8.0 Hz), 7.26-7.35 (3H, m), 7.35-7.44 (2H, m), 7.64-7.85 (5H, m), 8.95 (1H, d, J=8.2 Hz). Anal. Calcd for C21H15F3N4O: C, 63.63; H, 3.81; N, 14.14. Found: C, 63.46; H, 3.92; N, 13.98.

Aufarbeitung

  1. extractionextracted with AcOEt
  2. washwashed with brine
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customcrystallized with AcOEt/hexane
  7. temperatureThe mixture was heated
  8. temperatureto reflux for 15 h
  9. extractionextracted with AcOEt
  10. washwashed with saturated NaHCO3 aqueous solution
  11. dry with materialdried over Na2SO4
  12. filtrationfiltered
  13. concentrationconcentrated in vacuo
  14. custompurified by column chromatography on silica gel (hexane/AcOEt=50/50 to 0/100)
  15. customcrystallized with AcOEt/heptane

Quellen und Nachweise

ORD-Eintrag
ord-43bfa52f3235437691f8cd0873159a31
Quelldatensatz
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08435995B2

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