Sodium hydride → 4-Cyclopropylmethoxy-2-methylpyridine-1-oxide

HRID 327776

Reaktionsgleichung

Reaktionsgleichung von HRID 327776
[H-].[Na+].[CH3:3][C:4]1[CH:9]=[C:8]([N+]([O-])=O)[CH:7]=[CH:6][N+:5]=1[O-:13].[CH:14]1([CH2:17][OH:18])[CH2:16][CH2:15]1>>[CH:14]1([CH2:17][O:18][C:8]2[CH:7]=[CH:6][N+:5]([O-:13])=[C:4]([CH3:3])[CH:9]=2)[CH2:16][CH2:15]1

Komponenten

4

Edukt 3

HCID 24758Sodium hydrideHCID 75644Cyclopropanemethanol2×HCID 95291Pyridine, 2-methyl-4-nitro-, 1-oxide

Produkt 1

HCID 107024944-Cyclopropylmethoxy-2-methylpyridine-1-oxide

Reaktionsbedingungen

Temperatur
90 °C

Versuchsvorschrift

To sodium hydride (55% pure) (4.4 g, 0.1 mol) (washed with petroleum ether), cyclopropyl-methanol (50 ml) was added. Then a solution of 2-methyl-4-nitropyridine-N-oxide (6.5 g, 0.042 mol) in cyclopropylmethanol (30 ml) was added during about 1 h. The dark brown mixture was heated to 90° C. and stirred at 90° C. for about 1 h. Thereafter the cyclopropylmethanol was distilled off under reduced pressure and methylene chloride (100 ml) was added to the residue. The mixture was stirred for about 30 minutes, then filtered and concentrated which gave 9.5 g of crude material.

Aufarbeitung

  1. distillationThereafter the cyclopropylmethanol was distilled off under reduced pressure and methylene chloride (100 ml)
  2. additionwas added to the residue
  3. stirringThe mixture was stirred for about 30 minutes
  4. filtrationfiltered
  5. concentrationconcentrated which

Quellen und Nachweise

ORD-Eintrag
ord-73e7c7723bfe43eea292efd9bcfc5902
Quelldatensatz
uspto-grants-1993_12
Patentnummer
US05274099

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