反应详情

tert-Butyl piperazine-1-carboxylate (24.0 mg, 0.125 mmol) was added to a mixture of 4-chloro-2-(2-chloropyrimidin-4-yl)phenol (Preparation 874, 30.1 mg, 0.125 mmol), and triethylamine (61.2 uL, 0.437 mmol) in isopropyl alcohol (0.2 mL, 3 mmol). The reaction mixture was stirred at ambient temperature. After 18 hours, LC/MS analysis indicated the reaction was not complete. The reaction mixture was heated 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 sodium sulfate, filtered, and concentrated to give the product as a light brown paste (50 mg, 100%).

1. temperatureThe reaction mixture was heated 30 minutes at 70° C.
2. temperaturethen cooled to ambient temperature
3. washwashed with water
4. dry with materialbrine, dried over sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated
7. customto give the product as a light brown paste (50 mg, 100%)