反应详情

温度

90 °C

Step AA (2): To a solution of crude methyl 6-methoxy-2,3-dihydro-1H-inden-1-ol from Step AA (1) (24.3 g) in benzene (100 mL) was added pTSA (250 mg), and the resulting solution was heated at 90° C. for 3 h with a Dean-Stark trap to remove water. Saturated sodium bicarbonate was added, the aqueous layer was extracted with EtOAc (×3), and the combined organic layers were washed with brine, dried over anhydrous sodium sulfate, filtered, and evaporated. The crude product was distilled under vacuum to provide 5-methoxy-1H-indene as a colorless liquid (10 g). 1H NMR (400 MHz, CDCl3): 7.33 (1H, d), 6.96 (1H, d), 6.81 (1H, m), 6.75 (1H, m), 6.56 (1H, m), 3.82 (3H, s), 3.33 (2H, m).

1. customto remove water
2. additionSaturated sodium bicarbonate was added
3. extractionthe aqueous layer was extracted with EtOAc (×3)
4. washthe combined organic layers were washed with brine
5. dry with materialdried over anhydrous sodium sulfate
6. filtrationfiltered
7. customevaporated
8. distillationThe crude product was distilled under vacuum