반응 #55995

반응 방정식

4-acetylamino-5-chloro-2-methoxy-benzoyl azide

dichloromethane

1-benzylpiperazine

isocyanate

→

N-(4-acetylamino-5-chloro-2-methoxyphenyl)-4-benzylpiperazine-1-carboxamide

용매

—

petrol

toluene

반응 조건

후처리

1. 1
   workup.STIRRINGthe resulting solution stirred at room temperature for 1 hour
2. 2
   여과the precipitated solid filtered off
3. 3
   기타Recrystallisation from toluene

실험 절차

A solution of the 4-acetylamino-5-chloro-2-methoxy-benzoyl azide (e7) (1.35 g) in dry toluene (30 ml) was heated to 90° for 30 minutes with stirring under dry nitrogen until the evolution of nitrogen ceased. A dichloromethane solution of 1-benzylpiperazine (0.9 g) was then added to the cooled suspension of the isocyanate (e8) and the resulting solution stirred at room temperature for 1 hour. The reaction mixture was then poured into petrol (200 ml) and the precipitated solid filtered off. Recrystallisation from toluene give the N-(4-acetylamino-5-chloro-2-methoxyphenyl)-4-benzylpiperazine-1-carboxamide (e9) (1.4 g) m.p. 174°.

출처