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Sodium Bicarbonate → 3,4-Diethoxycarbonyl-2-fluoro-5-nitro-6-phenylpyridine

HRID 37492
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 37492
N[C:2]1[C:7]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[C:6]([C:13]([O:15][CH2:16][CH3:17])=[O:14])[C:5]([N+:18]([O-:20])=[O:19])=[C:4]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[N:3]=1.B(F)(F)[F:28].F.N([O-])=O.[Na+].C(=O)([O-])O.[Na+]>C(O)(=O)C.O>[CH2:11]([O:10][C:8]([C:7]1[C:2]([F:28])=[N:3][C:4]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)=[C:5]([N+:18]([O-:20])=[O:19])[C:6]=1[C:13]([O:15][CH2:16][CH3:17])=[O:14])=[O:9])[CH3:12]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 516892Sodium BicarbonateHCID 9855450Trifluoroborane HydrofluorideHCID 199356032-Amino-3,4-diethoxycarbonyl-5-nitro-6-phenylpyridineHCID 23668193Sodium Nitrite

Produkt 1

HCID 199356173,4-Diethoxycarbonyl-2-fluoro-5-nitro-6-phenylpyridine

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 176
Acetic Acid
Lösungsmittel
HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
-5 °C

Versuchsvorschrift

In 2 ml of acetic acid was dissolved 100 mg of 2-amino-3,4-diethoxycarbonyl-5-nitro-6-phenylpyridine, and 1.5 ml of 42% hydrofluoroboric acid was added to the solution. The mixture was cooled to -5° C., followed by adding dropwise a solution of 21 mg (1.1 eq) of sodium nitrite dissolved in 0.5 ml of water. Thirty minutes later, the temperature of the mixture was elevated to room temperature and the mixture was neutralized with sodium hydrogencarbonate, followed by extraction with ethyl acetate. After the organic layer was washed with water and a saturated aqueous solution of sodium chloride, and dried. After the solvent was distilled off, the resulting crystals (2-pyridone compound) were collected by filtration with hexane, and washed. The solvent was distilled off from the obtained filtrate, to give an oily substance.

Aufarbeitung

  1. additionwas added to the solution
  2. customThirty minutes
  3. customwas elevated to room temperature
  4. extractionfollowed by extraction with ethyl acetate
  5. washAfter the organic layer was washed with water
  6. dry with materiala saturated aqueous solution of sodium chloride, and dried
  7. distillationAfter the solvent was distilled off
  8. filtrationthe resulting crystals (2-pyridone compound) were collected by filtration with hexane
  9. washwashed
  10. distillationThe solvent was distilled off from the obtained filtrate
  11. customto give an oily substance

Quellen und Nachweise

ORD-Eintrag
ord-4afe1d8998b646889314d45135528e41
Quelldatensatz
uspto-grants-1995_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05420275

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