Phenylphosphonic dichloride → 2-Chloro-3,4-diethoxycarbonyl-6-methyl-5-nitropyridine

HRID 37476

Reaktionsgleichung

Reaktionsgleichung von HRID 37476
[CH2:1]([O:3][C:4]([C:6]1[C:7](=O)[NH:8][C:9]([CH3:20])=[C:10]([N+:17]([O-:19])=[O:18])[C:11]=1[C:12]([O:14][CH2:15][CH3:16])=[O:13])=[O:5])[CH3:2].C1(P(Cl)([Cl:30])=O)C=CC=CC=1>O>[Cl:30][C:7]1[C:6]([C:4]([O:3][CH2:1][CH3:2])=[O:5])=[C:11]([C:12]([O:14][CH2:15][CH3:16])=[O:13])[C:10]([N+:17]([O-:19])=[O:18])=[C:9]([CH3:20])[N:8]=1

Komponenten

4

Edukt 2

HCID 69990Phenylphosphonic dichlorideHCID 199355903,4-Diethoxycarbonyl-6-methyl-5-nitro-2-pyridone

Produkt 1

HCID 199355842-Chloro-3,4-diethoxycarbonyl-6-methyl-5-nitropyridine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
170 °C

Versuchsvorschrift

To 1.0 g of 3,4-diethoxycarbonyl-6-methyl-5-nitro-2-pyridone was added 1.3 ml (3.2 eq.) of phenylphosphonic dichloride. The mixture was heated at 170° C. for 20 mintues. Water was added to the reaction mixture, followed by extraction with ethyl acetate. The organic layer was washed with water and a saturated aqueous solution of sodium chloride and dried over magnesium sulfate. After the solvent was distilled off, the residue was purified by silica gel column chromatography (eluent:ethyl acetate) to give an oily product.

Aufarbeitung

  1. extractionfollowed by extraction with ethyl acetate
  2. washThe organic layer was washed with water
  3. dry with materiala saturated aqueous solution of sodium chloride and dried over magnesium sulfate
  4. distillationAfter the solvent was distilled off
  5. customthe residue was purified by silica gel column chromatography (eluent:ethyl acetate)
  6. customto give an oily product

Quellen und Nachweise

ORD-Eintrag
ord-1ee93671a1c449ee91ceaa24da712e78
Quelldatensatz
uspto-grants-1995_05
Patentnummer
US05420275

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