Reaktion #550869

ord-0e64e744c1024c63a60d7e7ad029bd55

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe dark red solution is evaporated, whereupon the residue
  2. 2
    Extraktionextracted with methylene chloride
  3. 3
    WaschenThe extract is washed with water
  4. 4
    Trocknendried over sodium sulfate
  5. 5
    Sonstigeevaporated
  6. 6
    Sonstigethe product is precipitated by the addition of ether
  7. 7
    FiltrationAfter filtration
  8. 8
    Waschenwashing with ether and petroleum ether
  9. 9
    Trocknenthe hygroscopic salt is dried over phosphorus pentoxide

Vorschrift

A mixture of 2.3 g of 9-chloro-1-nitroacridine, 1.65 g of N-methyl-N-(2-thiazolyl)hydrazine hydrochloride and 100 ml of dimethylformamide is stirred at room temperature for about 18 hours. The dark red solution is evaporated, whereupon the residue is made alkaline with sodium carbonate solution and extracted with methylene chloride. The extract is washed with water, dried over sodium sulfate and evaporated. The residue is taken up in ethanol, acidified with ethanolic hydrochloric acid and the product is precipitated by the addition of ether. After filtration and washing with ether and petroleum ether, the hygroscopic salt is dried over phosphorus pentoxide. There is obtained 1-nitro-9-acridanone methyl (2-thiazolyl)hydrazone hydrochloride of melting point 185° (decomposition).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04544659uspto-grants-1985_10