反应详情

Reduced iron (6.7 g), ammonium chloride (0.53 g) and acetic acid (0.57 ml) were added to a mixed solvent of 2-propanol (40 ml) and water (8 ml), and the resulting mixture was heated over a steam bath and refluxed. To the mixture was further added the Nitro Compound (C) obtained in the step (3) above (6.27 g) and the reflux was further continued for 30 minutes. Sodium hydroxide (3.0 g) was dissolved in water (30 ml) and this solution was added to the above mixture. The resulting mixture was stirred and then filtered to remove insolubles. To the filtrate was added water (100 ml) and acetic acid (5 ml) and the resultant mixture was stirred. The resulting precipitated crystals were filtered and washed with water and dried to obtain 5.37 g (95%) of Amino Compound (D) as pale orange crystals (m.p.: 143.5°-144.5° C.).

1. temperaturethe resulting mixture was heated over a steam bath
2. temperaturerefluxed
3. customobtained in the step (3) above (6.27 g)
4. additionthis solution was added to the above mixture
5. filtrationfiltered
6. customto remove insolubles
7. additionTo the filtrate was added water (100 ml) and acetic acid (5 ml)
8. stirringthe resultant mixture was stirred
9. customThe resulting precipitated crystals
10. filtrationwere filtered
11. washwashed with water
12. customdried