反应详情

温度

-78 °C

To a solution of diisopropylamine (5.2 mL, 36.9 mmol), in THF (20 mL) is added n-BuLi (14.8 mL, 36.9 mmol, 2.5 M in hexane) at −78° C. After 30 min, 5-methoxyindan-1-one (5.0 g, 30.8 mmol) in THF (35 mL) is added. After it is stirred at −78° C. for 1 h, the mixture is warmed to 10° C. for 30 min. The mixture is cooled again to −78° C. and methyl iodide (2.3 mL, 36.9 mmol) is added. The mixture is then warmed to RT over 1 h. NH4Cl solution is added and extracted with EtOAc. The organic extract is dried with MgSO4, concentrated and purified by chromatography to give the title compound (2.38 g): (M+H)+=177.

1. temperaturethe mixture is warmed to 10° C. for 30 min
2. temperatureThe mixture is cooled again to −78° C.
3. temperatureThe mixture is then warmed to RT over 1 h
4. extractionextracted with EtOAc
5. extractionThe organic extract
6. dry with materialis dried with MgSO4
7. concentrationconcentrated
8. custompurified by chromatography