反应详情

To a solution of methyl 2-(2-tert-butoxy-2-oxoethyl)-2,3-dihydro-1H-indene-2-carboxylate (4.5 g, 15.50 mmol) in EtOH/THF (70 mL, 1:1) at room temperature was added 1 M sodium hydroxide (35 ml, 35.0 mmol), and the mixture was stirred at room temperature for 1.5 hour. To the reaction mixture was added DCM and acidified by 1 M HCl to pH=7. The mixture was extracted with DCM, and the combined organic layer was washed with brine and dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure. The obtained residue was purified by flash chromatography (silica gel, 10 to 30% EtOAc/HEP) and gave the title compound: 1.4 g (yield: 15%). LCMS (condition B): 275.2 (M−1); retention time=1.17 min.

1. extractionThe mixture was extracted with DCM
2. washthe combined organic layer was washed with brine
3. dry with materialdried over anhydrous sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. customThe obtained residue was purified by flash chromatography (silica gel, 10 to 30% EtOAc/HEP)