反应详情

温度

95 °C

Hexamethylentetramine (197 mg, 1.4 mmol) was added to a solution of compound 4-(2,6-dibromo-3-methyl-4-nitrophenoxy)-2-isopropylphenol of Part 8C (250 mg, 0.56 mmol) and TFA (5 mL). The resulting reaction mixture was stirred for 16 hours at 95° C. The reaction mixture was cooled to room temperature and 1N HCl (10 mL) was added. After another hour of stirring, the reaction mixture was extracted with EtOAc (3×30 mL), the combined organic phases washed by 1N HCl (15 mL), H2O (20 mL) and brine (20 mL). After drying over Na2SO4, concentration and filtration through a pad of silica, 210 mg (79%) of 5-(2,6-dibromo-3-methyl-4-nitrophenoxy)-2-hydroxy-3-isopropylbenzaldehyde was obtained as a light yellow solid.

1. customThe resulting reaction mixture
2. temperatureThe reaction mixture was cooled to room temperature
3. stirringAfter another hour of stirring
4. extractionthe reaction mixture was extracted with EtOAc (3×30 mL)
5. washthe combined organic phases washed by 1N HCl (15 mL), H2O (20 mL) and brine (20 mL)
6. dry with materialAfter drying over Na2SO4, concentration and filtration through a pad of silica