反应详情

To a solution of 7-(4-fluorophenyl)-7-(2-hydroxy-3,4,6-trimethylphenyl)heptanoic acid (1.32 g) in acetic acid (10 ml) was added dropwise a solution of bromine (0.19 ml) in acetic acid (2 ml) with ice cooling. After completion of addition, the mixture was stirred at room temperature for 30 minutes. The reaction mixture was extracted by addition of water and ethyl acetate. The organic layer was separated and washed in turn with water and saturated saline and dried with anhydrous magnesium sulfate and the solvent was distilled off under reduced pressure. The residue was recrystallized from ethyl acetate/hexane to obtain 7-(5-bromo-2-hydroxy-3,4,6-trimethylphenyl)-7-(4-fluorophenyl)heptanoic acid (1.04 g) (Compound 12). The physical properties and spectrum data thereof are shown in Tables 3 and 4.

1. additionAfter completion of addition
2. extractionThe reaction mixture was extracted by addition of water and ethyl acetate
3. customThe organic layer was separated
4. washwashed in turn with water and saturated saline
5. dry with materialdried with anhydrous magnesium sulfate
6. distillationthe solvent was distilled off under reduced pressure
7. customThe residue was recrystallized from ethyl acetate/hexane