反应详情

Pyridine (0.255 mL; 3.15 mmol) was added to a stirred solution of amino-3-[2-(4-cyanophenyl)ethoxy]benzene (0.15 g; 0.629 mmol; from step (ii) above) and 2-chlorobenzenesulfonyl chloride (0.173 mL; 0.818 mmol) in CH2Cl2 (4 mL). After 45 minutes at room temperature the solvent was removed in vacuo. To remove traces of pyridine, EtOH was added and evaporated. The residue was partitioned between water and EtOAc. The organic layer was washed with 0.1M aqueous HCl and brine, dried (Na2SO4) and the solvent removed in vacuo. Purification by flash chromatography (SiO2; toluene:EtOAc (1:0 to 9:1)) afforded 0.095 g (35%) of the sub-title compound.

1. customAfter 45 minutes at room temperature the solvent was removed in vacuo
2. customTo remove traces of pyridine, EtOH
3. additionwas added
4. customevaporated
5. customThe residue was partitioned between water and EtOAc
6. washThe organic layer was washed with 0.1M aqueous HCl and brine
7. dry with materialdried (Na2SO4)
8. customthe solvent removed in vacuo
9. customPurification by flash chromatography (SiO2; toluene:EtOAc (1:0 to 9:1))