反应详情

温度

90 °C

6-Hydroxy-1-oxo-3-phenyl-1H-indene-2-carboxylic acid methyl ester (2.6 g, 9.28 mmol) obtained in Step 1 was dissolved in dichloroethane, and boron tribromide methyl sulfide (6.0 mL, 27.84 mmol) was added thereto. The mixture was refluxed for 2 hrs at 90° C., cooled in an ice bath, neutralized using sodium bicarbonate, and adjusted to pH 2 using 6N hydrochloric acid. The resulting mixture washed successively with dichloromethane and water. The organic layer was separated, dried over anhydrous MgSO4, concentrated under a reduced pressure and recrystallized to obtain 1.2 g of the titled compound (yield: 48.6%).

1. temperaturecooled in an ice bath
2. washThe resulting mixture washed successively with dichloromethane and water
3. customThe organic layer was separated
4. dry with materialdried over anhydrous MgSO4
5. concentrationconcentrated under a reduced pressure
6. customrecrystallized