反应详情

Solid 2-nitro-3-methylanisole (20 g) is added portion to a hot (40°-60° C.) suspension of iron (30 g) in 20% acetic acid (400 ml). The mixture is heated on a steam bath for 40 min, filtered still hot and neutralized (after cooling) with 50% aqueous sodium hydroxide. The mixture is steam distilled (2 liters of water collected). The distillate is extracted with diethyl ether and the etheral solution is dried and evaporated to give an oily residue of 2-methoxy-6-methylbenzenamine: nmr (CDCl3) δ2.15 (s, 3H), 3.7 (s, 2H), 3.8 (s, 3H) and 6.7 (m, 3H).

1. temperatureThe mixture is heated on a steam bath for 40 min
2. filtrationfiltered still hot
3. temperatureneutralized (after cooling) with 50% aqueous sodium hydroxide
4. distillationdistilled
5. custom(2 liters of water collected)
6. extractionThe distillate is extracted with diethyl ether
7. customthe etheral solution is dried
8. customevaporated