反应详情

A solution of 3-chloro-6-(4-methoxy-phenyl)-pyridazine (Step 1, 2.5 g, 0.0113 mol) in 1 M BBr3/CH2Cl2 (34 mL) was stirred at RT for 16 h. The solution was 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. The solid was washed with 50% EtOAc/hexane mixture to give the title compound as a yellow solid MS (ESI pos. ion) m/z: 207.2(M+H). Calc'd Exact Mass for C10H7ClN2O: 206.63.

1. concentrationThe solution was 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
6. washThe solid was washed with 50% EtOAc/hexane mixture