反应详情

温度

98 °C

4-(2,6-dibromo-4-nitro-3-trifluoromethylphenoxy)-2-isopropylphenol of Part 11C (220 mg, 0.44 mmol) was dissolved in TFA (3 mL) and hexamethylenetetramine (154 mg, 1.1 mmol) was added to the reaction. The reaction mixture was heated at 98° C. for 12 hours, cooled down and 1N HCl (4 mL) was added. The reaction mixture was stirred for 5 hours at room temperature, extracted with EtOAc, washed with H2O, NaHCO3 and brine. The organic layer was dried by MgSO4 and concentrated. The residue was purified on column (silica gel, gradient elution with n-heptane/EtOAc) to give 130 mg (57%) of 5-(2,6-dibromo-4-nitro-3-trifluoromethylphenoxy)-2-hydroxy-3-isopropylbenzaldehyde.

1. temperaturecooled down
2. extractionextracted with EtOAc
3. washwashed with H2O, NaHCO3 and brine
4. dry with materialThe organic layer was dried by MgSO4
5. concentrationconcentrated
6. customThe residue was purified on column (silica gel, gradient elution with n-heptane/EtOAc)