反应详情

温度

125 °C

To a stirred solution of 4-(4-fluoro-2-(tetrahydro-2H-pyran-4-yloxy)phenylamino)-5-methylthieno[2,3-d]pyrimidine-6-carbonitrile (0.036 g, 0.093 mmol) in DMF (1.0 mL) was added sodium azide (0.012 g, 0.18 mmol) and ammonium chloride (0.01 g, 0.18 mmol) and the mixture heated at 125° C. for 1.5 hours. The solvent was concentrated in vacuo and the residue co-evaporated with toluene. The crude product was dissolved in 10% MeOH in DCM and the insoluble material removed by filtration. The residue was triturated from MeCN, the solid collected and dried under vacuum. The solid was purified by reverse phase preparative HPLC to give the product as beige solid after lyophilisation (0.021 g, 54%).

1. concentrationThe solvent was concentrated in vacuo
2. dissolutionThe crude product was dissolved in 10% MeOH in DCM
3. customthe insoluble material removed by filtration
4. customThe residue was triturated from MeCN
5. customthe solid collected
6. customdried under vacuum
7. customThe solid was purified by reverse phase preparative HPLC