反应详情

To a solution of tert-butyl 3-(7-(bis((2-(trimethylsilyl)ethoxy)methyl)amino)pyrazolo[1,5-a]pyrimidin-5-yl)pyrrolidine-1-carboxylate 3.95 g, 7.0 mmol) in CH3CN (30 mL) was added NIS (1.65 mg, 7.0 mmol). The mixture was stirred at rt for 2 h and diluted with EtOAC (50 mL) and washed with saturated sodium thiosulfate, dried over Na2SO4, filtered and concentrated in vacuo. The residue was purified by Biotage (CH2Cl2/EtOAc, 100:1 to 10:1) to the title compound as a light brown oil. LC/MS RT=2.49 min. Mass calculated for, M+H 689.23, observed 389.17.

1. additiondiluted with EtOAC (50 mL)
2. washwashed with saturated sodium thiosulfate
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customThe residue was purified by Biotage (CH2Cl2/EtOAc, 100:1 to 10:1) to the title compound as a light brown oil