반응 #342733

반응 방정식

methylamine

4-hydroxy-3-nitroquinoline

phosphorus oxychloride

→

4-methylamino-3-nitroquinoline

용매

water

N,N-dimethylformamide

반응 조건

후처리

1. 1
   온도The solution was heated on a steam bath for 5 minutes
2. 2
   workup.ADDITIONpoured
3. 3
   온도The mixture was heated on a steam bath for fifteen minutes
4. 4
   기타The solid was separated by filtration
5. 5
   workup.DISSOLUTIONdissolved in dilute hydrochloric acid
6. 6
   여과The solution was filtered
7. 7
   기타The solid precipitate was separated by filtration
8. 8
   세척washed with water
9. 9
   기타dried

실험 절차

To a solution of 5.7 g (0.30 mole) of 4-hydroxy-3-nitroquinoline in 50 ml of N,N-dimethylformamide was added 9.3 g (0.60 mole) of phosphorus oxychloride. The solution was heated on a steam bath for 5 minutes, then poured with stirring into 200 ml of 40% aqueous methylamine. The mixture was heated on a steam bath for fifteen minutes, then diluted with 200 ml of water. The solid was separated by filtration, then dissolved in dilute hydrochloric acid. The solution was filtered and the filtrate was basified with ammonium hydroxide. The solid precipitate was separated by filtration, washed with water and dried to provide Yellow solid 4-methylamino-3-nitroquinoline, m.p. 167°-171° C.

출처