反应详情

A reaction solution consisting of 5.66 g. (0.03 mole) 6-chloro-4-nitro-2-picoline-1-oxide and 100 ml. ethanol was saturated with anhydrous ammonia and sealed in a strong bottle. This reaction mixture was heated and maintained at a temperature in the range of 100° to 105° C. for 21 hrs. The bottle and contents were then cooled and the seal was broken. Crystals had formed. The crystals were collected on a filter and washed with a small amount of cold ethanol. Recrystallization from 95% aqueous ethanol yielded 2.06 g. (41% yield) of 6-amino-4-nitro-2-picoline-1-oxide as yellow needles having a melting point at 221° to 222° C. (with decomposition). When a small sample was mixed with ethanolic ferric chloride a blue solution was obtained.

1. customsealed in a strong bottle
2. temperatureThis reaction mixture was heated
3. temperaturemaintained at a temperature in the range of 100° to 105° C. for 21 hrs
4. temperatureThe bottle and contents were then cooled
5. customCrystals had formed
6. customThe crystals were collected on
7. filtrationa filter
8. washwashed with a small amount of cold ethanol
9. customRecrystallization from 95% aqueous ethanol
10. customyielded 2.06 g