反应详情

A solution of 1,3,5-trifluorobenzene (318 mg, 2.41 mmol) in tetrahydrofuran (6.0 mL) was cooled to 78° C. under nitrogen, and thereto was added dropwise 2N lithium diisopropylamide (1.53 mL, 3.06 mmol), and the mixture was stirred for 30 minutes, Then, thereto was added dropwise a solution of the compound of Example 1-1 (650 mg, 1.34 mmol) in tetrahydrofuran (16 mL), and the mixture was stirred at −78° C. for 3 hours. To the reaction solution was added saturated aqueous sodium bicarbonate, and the mixture was extracted with ethyl acetate, dried over magnesium sulfate and filtered. The filtrate was evaporated and purified by silica gel column chromatography (hexane/ethyl acetate/ammonia water=50/1/0.25 to 30/1/0.16 to 20/1/0.1) to give the titled compound (223 mg, 27%).

1. stirringthe mixture was stirred at −78° C. for 3 hours
2. extractionthe mixture was extracted with ethyl acetate
3. dry with materialdried over magnesium sulfate
4. filtrationfiltered
5. customThe filtrate was evaporated
6. custompurified by silica gel column chromatography (hexane/ethyl acetate/ammonia water=50/1/0.25 to 30/1/0.16 to 20/1/0.1)