반응 #95061

반응 방정식

4-fluorophenylhydrazine hydrochloride

N-(3-oxocyclohexyl)acetamide

→

title compound

N-(6-fluoro-1,3,4,9-tetrahydro-2H-carbazol-2-yl)acetamide

용매

HOAc

반응 조건

후처리

1. 1
   온도heated on the steam bath
2. 2
   기타At 80°-90° an exothermic reaction
3. 3
   온도the source of heat
4. 4
   기타was removed until the temperature
5. 5
   기타had fallen to 85°
6. 6
   workup.ADDITIONthe warm mixture was poured into H2O
7. 7
   기타the gummy insolubles triturated until solid
8. 8
   세척The filtered solid was washed thoroughly with H2O
9. 9
   기타The crude product was recrystallized from ethanol

실험 절차

A mixture of 0.05 mol of 4-fluorophenylhydrazine hydrochloride and 0.05 mol of N-(3-oxocyclohexyl)acetamide in 75 ml of glacial HOAc was stirred and heated on the steam bath. At 80°-90° an exothermic reaction occurred and the source of heat was removed until the temperature had fallen to 85°. After an additional 4-5 hr at 85°-90°, the warm mixture was poured into H2O and the gummy insolubles triturated until solid. The filtered solid was washed thoroughly with H2O and then with Et2O until the washings were essentially colorless. The crude product was recrystallized from ethanol to give the title compound, mp 209°-210°.

출처