Reaktion #455475

Reaktionsgleichung

5,6-Dichloro-N-hydroxy-3-pyridinecarboximidoyl chloride

triethylamine

1-butyne

→

desired product

Ausbeute 90.0%

3-(2,3-Dichloro-5-pyridyl)-5-ethylisoxazole

Ausbeute 90.0%

Lösungsmittel

ether

ether

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigewas bubbled through the reaction mixture
2. 2
   Filtrationfiltered
3. 3
   Sonstigethe filtrate evaporated to dryness under reduced pressure
4. 4
   SonstigeRecrystallisation of the residue from hexane

Vorschrift

5,6-Dichloro-N-hydroxy-3-pyridinecarboximidoyl chloride (0.85 g, 3.8 mmol) was dissolved with stirring in ether (60 mL) and a solution of triethylamine (0.8 g, 7.9 mmol) in ether (50 mL) added dropwise to the solution while 1-butyne was bubbled through the reaction mixture. The mixture was stirred at room temperature overnight, filtered, and the filtrate evaporated to dryness under reduced pressure. Recrystallisation of the residue from hexane gave the desired product (0.83 g, 90%) as a cream solid, melting point. 98-9° C.

Quelle