반응 #54397

반응 방정식

4,4-dibromo-3-methyl-1-(4-sulfophenyl)-2-pyrazolin-5-one

2-hydrazinopyridine

HCl

→

3-Methyl-4-(2-pyridylazo)-1-(4-sulfophenyl)-2-pyrazolin-5-one

용매

water

반응 조건

후처리

1. 1
   온도The mixture was heated on the steam bath a total of six hours
2. 2
   온도After a few minutes of heating
3. 3
   온도The mixture was cooled somewhat
4. 4
   기타the orange solid was isolated by suction filtration
5. 5
   세척After washing once with tetrahydrofuran, twice with ether
6. 6
   기타drying

실험 절차

41.0 g (0.10 mole) of 4,4-dibromo-3-methyl-1-(4-sulfophenyl)-2-pyrazolin-5-one, which can be prepared according to the method of Machiele, U.S. Pat. No. 3,952,009 (Example 1), and 16.0 g (0.15 mole) of 2-hydrazinopyridine were combined in 180 ml of water. The mixture was heated on the steam bath a total of six hours. After a few minutes of heating, the solution goes to a very thick slurry. The mixture was cooled somewhat, 10 ml of concentrated HCl were added, and the orange solid was isolated by suction filtration. After washing once with tetrahydrofuran, twice with ether, and drying, the yield of dye was 17.8 g (50 percent).

출처