반응 #455475

반응 방정식

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

triethylamine

1-butyne

→

desired product

수율 90.0%

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

수율 90.0%

용매

ether

ether

반응 조건

후처리

1. 1
   기타was bubbled through the reaction mixture
2. 2
   여과filtered
3. 3
   기타the filtrate evaporated to dryness under reduced pressure
4. 4
   기타Recrystallisation of the residue from hexane

실험 절차

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.

출처