Reaktion #49924

ord-70c0923c5e2848879bce03b94ac269c2

Lösungsmittel

Reaktionsbedingungen

Temperatur
23°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionthe mixture was extracted with ether
  2. 2
    ExtraktionA second extraction
  3. 3
    Trocknenthe combined organic extracts were dried over magnesium sulfate
  4. 4
    SonstigeEvaporation

Vorschrift

A solution of N'-t-butyl-N-(2-pyridinecarbonyl)-hydrazine (1.0 g, 0.00518 mol) in 20 ml of toluene was treated dropwise simultaneously with a solution of sodium hydroxide (1.24 g of 50% aqueous solution) in 5 ml of water and 2-nitrobenzoyl chloride (0.96 g). The resulting mixture was stirred at 23° C. overnight. Water was added and the mixture was extracted with ether. A second extraction was performed with methylene chloride and the combined organic extracts were dried over magnesium sulfate. Evaporation afforded 0.4 g of N'-t-butyl-N-(2-pyridinecarbonyl)-N'-(2-nitrobenzoyl)hydrazine as a yellow solid: m.p. 137°-140° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05424333uspto-grants-1995_06