反应详情

温度

200 °C

To a 20 mL scintillation vial was charged 5-chloro-3-(quinolin-3-yl)-N,N-bis((2-(trimethylsilyl)-ethoxy)methyl)pyrazolo[1,5-a]pyrimidin-7-amine (0.09 mmol, 50 mg), NMP (1 mL), N,N-diisopropylethylamine (0.36 mmol, 63 μL), and 4-N-Boc-piperazine (0.27 mmol, 50 mg). The resulting solution was heated to 200° C. in microwave synthesizer for 30 minutes. Upon completion, the NMP was removed in vacuo as an azeotrope using chlorobenzene. This residue was dissolved in acetonitrile (1 mL) to which N-bromosuccinimide (0.10 mmol, 17.7 mg) was added. This reaction mixture was allowed to stir at room temperature for 2 hours. The reaction mixture was concentrated in vacuo and tert-butyl 4-(7-amino-6-bromo-3-(quinolin-3-yl)pyrazolo[1,5-a]pyrimidin-5-yl)piperazine-1-carboxylate used without further purification.

1. customUpon completion, the NMP was removed in vacuo as an azeotrope
2. additionwas added
3. concentrationThe reaction mixture was concentrated in vacuo and tert-butyl 4-(7-amino-6-bromo-3-(quinolin-3-yl)pyrazolo[1,5-a]pyrimidin-5-yl)piperazine-1-carboxylate
4. customused without further purification