反应详情

温度

60 °C

A mixture of 5-[2-fluoro-6-hydroxy-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-phenyl]-1,1-dioxo-1,2,5-thiadiazolidin-3-one (150 mg, 0.325 mmol) and Pd(PPh3)4 (38 mg, 0.0325 mmol) in DME (2 mL) is heated at 60° C. under argon for 1 h. Then methanesulfonic acid 2-bromomethyl-5-methylphenyl ester (181 mg, 0.65 mmol) and Na2CO3 (2N solution, 0.81 mL) is added. The mixture is heated at 120° C. in a microwave for 20 min. 1N HCl is added and the reaction mixture is extracted with EtOAc. The organic layer is washed with brine, dried over MgSO4 and filtered. The filtrate is concentrated to give the title compound and it is used directly in the next step: MS (M−H)−=533.

1. temperatureThe mixture is heated at 120° C. in a microwave for 20 min
2. extractionthe reaction mixture is extracted with EtOAc
3. washThe organic layer is washed with brine
4. dry with materialdried over MgSO4
5. filtrationfiltered
6. concentrationThe filtrate is concentrated