반응 #54148

반응 방정식

2-chloro-5-nitropyridine

hydrazine

→

2-Hydrazino-5-nitropyridine

용매

methanol

water

반응 조건

후처리

1. 1
   workup.ADDITIONwas added
2. 2
   기타a greenish-yellow precipitate separated
3. 3
   온도at reflux for 30 minutes
4. 4
   여과The greenish solid was filtered off
5. 5
   세척washed with cold methanol
6. 6
   세척washed
7. 7
   기타vacuum dried

실험 절차

To a slurry of 47.6 g (0.3 mol) of 2-chloro-5-nitropyridine in a mixture of 400 ml methanol and 60 ml water and cooled to 10° C. was added with cooling below 30° 86 g hydrazine (95 percent) over about 10 minutes. The solids first went into solution, then a greenish-yellow precipitate separated. The mixture was stirred at reflux for 30 minutes. The greenish solid was filtered off and washed with cold methanol. The solid was slurried in 200 ml of cold water, washed and vacuum dried. The yield was 40.1 g (87 percent).

출처