반응 #72711

반응 방정식

phthalic anhydride

N,N-dimethyl hydrazine dihydrochloride

diethyl-phenyl-amine

→

desired product

수율 85.0%

2-Dimethylamino-isoindole-1,3-dione

수율 85.0%

용매

toluene

반응 조건

후처리

1. 1
   workup.ADDITIONwere added
2. 2
   온도The reaction mixture was refluxed for 18 hours
3. 3
   기타while removing the formed water via a Dean-Stark trap
4. 4
   기타Then, toluene was evaporated under reduced pressure
5. 5
   기타the resulting crude was purified on silica gel chromatography with (1:5) EtOAc

실험 절차

To the suspension of phthalic anhydride (62.5 mmol) in toluene (500 ml), N,N-dimethyl hydrazine dihydrochloride (50 mmol) and diethyl-phenyl-amine (90 mmol) were added. The reaction mixture was refluxed for 18 hours while removing the formed water via a Dean-Stark trap. Then, toluene was evaporated under reduced pressure and the resulting crude was purified on silica gel chromatography with (1:5) EtOAc:dichloromethane, to give the desired product in 85% yield.

출처