반응 #1328405

반응 방정식

2,7-Dinitro-9-fluorenone

hydrochloric acid

→

2,7-Diamino-9-fluorenone

용매

acetic acid

반응 조건

후처리

1. 1
   온도refluxed for 1 hour
2. 2
   여과The solid was harvested by filtration
3. 3
   세척The solid was washed first with concentrated hydrochloric acid
4. 4
   workup.DISSOLUTIONThe residue was dissolved
5. 5
   여과The solution was filtered
6. 6
   세척The precipitate was washed with water
7. 7
   기타dried
8. 8
   기타recrystallized from dioxane
9. 9
   기타to be 284–286° C.

실험 절차

2,7-Dinitro-9-fluorenone (162 g, 0.6 mol, from Aldrich) was added cautiously to a solution of hydrated stannous chloride (1100 g, 4.9 mol, from Aldrich) in a mixture of concentrated hydrochloric acid (900 ml) and acetic acid (1600 ml). The suspension was stirred and refluxed for 1 hour. The mixture was cooled to room temperature, and a solid appeared. The solid was harvested by filtration. The solid was washed first with concentrated hydrochloric acid, and then with water until the filtrate color was violet. The residue was dissolved in boiling water. The solution was filtered and then made alkaline with sodium hydroxide to from a precipitate. The precipitate was washed with water, dried, and recrystallized from dioxane. The yield of 2,7-diamino-9-fluorenone was 108 g (85.7%). The melting point was found to be 284–286° C.

출처