反应详情

tert-Butyl piperazine-1-carboxylate (24.0 mg, 0.13 mmol) was added to a mixture of 4-chloro-2-(2-chloropyrimidin-4-yl)phenol (Preparation 1, 30.1 mg, 0.13 mmol), and triethylamine (61.2 uL, 0.44 mmol) in isopropyl alcohol (0.2 mL). The reaction mixture was stirred at ambient temperature. After 18 hours, LCMS analysis indicated the reaction was not complete. The reaction mixture was heated for 30 minutes at 70° C. then cooled to ambient temperature. The reaction mixture was diluted with ethyl acetate, washed with water then brine, dried over anhydrous sodium sulfate, filtered, and concentrated in vacuo to afford the title compound as a light brown paste (50 mg).

1. temperatureThe reaction mixture was heated for 30 minutes at 70° C.
2. temperaturethen cooled to ambient temperature
3. washwashed with water
4. dry with materialbrine, dried over anhydrous sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated in vacuo