반응 #55655

반응 방정식

3-nitro-4-chloro-benzophenone

diisobutylamine

→

3-nitro-4-(N,N-diisobutylamino)-benzophenone

용매

ethanol

ethanol

반응 조건

후처리

1. 1
   workup.DISTILLATIONis distilled off under reduced pressure, and 260 ml
2. 2
   workup.ADDITIONof petroleum ether (b.p.: 40° to 100° C.) are added to the solid residue
3. 3
   기타The separated diisobutylamine hydrochloride is removed by filtration
4. 4
   기타the filtrate is evaporated
5. 5
   기타the residue is recrystallized from ethanol

실험 절차

A mixture of 26 g of 3-nitro-4-chloro-benzophenone, 20 ml. of ethanol and 35 ml. of diisobutylamine is heated to 80° to 85° C. under stirring, and the reaction mixture is kept at this temperature for 6 hours. When the reaction is over, the ethanol is distilled off under reduced pressure, and 260 ml. of petroleum ether (b.p.: 40° to 100° C.) are added to the solid residue. The separated diisobutylamine hydrochloride is removed by filtration, the filtrate is evaporated, and the residue is recrystallized from ethanol. 32.7 g of 3-nitro-4-(N,N-diisobutylamino)-benzophenone are obtained, m.p. 80°-81° C. (compound B9 supra)

출처