反应详情

A solution of 3-benzyl-6-(3-fluoro-4-methoxy-phenyl)-pyridazine (Step 2, 1.5 g, 5.1 mmol) in 25 mL of 1 M BBr3/CH2Cl2 was stirred at RT for 16 h. The solution was then concentrated in vacuo and the residue was re-dissolved in 100 mL of EtOAc. The organic phase was washed with 40 mL of water followed by 40 mL of brine, dried over Na2SO4 and concentrated in vacuo to give the title compound. The solid has poor solubility in EtOAc and CH2Cl2 and was washed with 50% EtOAc/hexane and then used in the next step (yellow solid). MS (ESI pos. ion) m/z: 281.3 (M+H). Calc'd Exact Mass for C17H13FN2O: 280.30.

1. concentrationThe solution was then concentrated in vacuo
2. dissolutionthe residue was re-dissolved in 100 mL of EtOAc
3. washThe organic phase was washed with 40 mL of water
4. dry with materialdried over Na2SO4
5. concentrationconcentrated in vacuo