反应详情

To 1-Bromo-4-isopropoxy-2-methyl-5-nitro-benzene from the previous step (0.734 g, 2.68 mmol) and iron (powder, 325 mesh, 1.05 g) in 20 mL ethanol is added 1 mL of 1N aqueous HCl with cooling in an ice bath. Following this addition, the reaction is heated at reflux for 2 hrs. Then an additional 0.5 g of iron is added and the reaction is heated at reflux for an additional 2 hrs. The reaction mixture is cooled down and filtered though a pad of Celite. The filtrate is concentrated in vacuo, affording 5-Bromo-2-isopropoxy-4-methyl-phenylamine as an orange oil. The product is used for the next step without further purification.

1. temperaturewith cooling in an ice bath
2. additionthis addition
3. temperaturethe reaction is heated
4. temperatureat reflux for 2 hrs
5. temperaturethe reaction is heated
6. temperatureat reflux for an additional 2 hrs
7. temperatureThe reaction mixture is cooled down
8. filtrationfiltered though a pad of Celite
9. concentrationThe filtrate is concentrated in vacuo