反应详情

温度

-78 °C

According to Scheme 3, step 1: to a solution of 4,6-difluoro-indan-1-one (5.0 g, 29.8 mmol) in dry tetrahydrofuran (100 ml) at −78° C. a 2M solution of lithiumdiisopropylamide (16.4 ml, 32.7 mmol) in tetrahydrofuran was added dropwise and the mixture was stirred for 1 h at −78° C. Then iodomethane (4.64 g, 32.7 mmol) was added and the mixture was slowly warmed to 25° C. After addition of aqueous saturated NaHCO3 the mixture was extracted 3 times with ethyl acetate. The combined organic layers were dried over Na2SO4 and filtered, solvents were evaporated in vacuo. The crude product was purified by silica gel chromatography (eluting with 0% to 100% ethyl acetate in heptane to give 1.15 g of 4,6-Difluoro-2-methyl-indan-1-one (7a).

1. temperaturethe mixture was slowly warmed to 25° C
2. extractionwas extracted 3 times with ethyl acetate
3. dry with materialThe combined organic layers were dried over Na2SO4
4. filtrationfiltered
5. customsolvents were evaporated in vacuo
6. customThe crude product was purified by silica gel chromatography (
7. washeluting with 0% to 100% ethyl acetate in heptane