反应详情

4-(2,6-Dibromo-4-nitro-3-trifluoromethylphenoxy)-2-methyl-6-isopropylphenol of Part 11E (120 mg, 0.23 mmol) was dissolved in EtOH (5 mL) and sodium hydrosulfite (204 mg, 1.2 mmol) was added. The reaction mixture was heated at reflux for 48 hours. The reaction progress was monitored by TLC (n-heptane/EtOAc 65:35) and when complete diluted with EtOAc. The organic phase was washed with water, brine, dried over MgSO4 and concentrated. The residue was purified on column (silica gel, gradient elution with n-heptane/EtOAc) to give 90 mg (81%) of 4-(4-amino-2,6-dibromo-3-trifluoromethylphenoxy)-2-methyl-6-isopropylphenol.

1. temperatureThe reaction mixture was heated
2. temperatureat reflux for 48 hours
3. washThe organic phase was washed with water, brine
4. dry with materialdried over MgSO4
5. concentrationconcentrated
6. customThe residue was purified on column (silica gel, gradient elution with n-heptane/EtOAc)