反应详情

To a solution of 180 mg (0.711 mmol) [6-chloro-4-(2-chloro-phenyl)-pyridin-3-yl]-methyl-amine in 7 ml dry tetrahydrofuran 0.86 ml of a 0.91 M solution (0.78 mmol) of potassium hexamethyldisilazide in tetrahydrofuran was added at room temperature under an atmosphere of argon. After 45 min 295 mg (0.924 mmol) 2-(3,5-bis-trifluoromethyl-phenyl)-2-methyl-propionyl chloride were added. The reaction mixture was stirred at room temperature for 3 h. Quenching with water was followed by dilution with tert-butyl methyl ether and washing with 2 M aqueous sodium carbonate solution and brine. The combined aqueous layers were extracted with two portions of tert-butyl methyl ether. The combined organic extracts were dried with sodium sulfate and concentrated. Flash chromatography gave 254 mg (67%) of the title compound as a light yellow solid.

1. customQuenching with water
2. washwashing with 2 M aqueous sodium carbonate solution and brine
3. extractionThe combined aqueous layers were extracted with two portions of tert-butyl methyl ether
4. dry with materialThe combined organic extracts were dried with sodium sulfate
5. concentrationconcentrated