反应详情

To a stirred solution of {4-[4-(3-Pyrrolidin-1-ylpropoxy)phenyl]tetrahydropyran-4-yl}methylamine (320 mg, 1.0 mmol) in acetonitrile (˜5 mL), was added Hunig's base (190 μL, 1.1 mmol, 1.1 eq.) and 2-chloro-3-nitropyridine (175 mg, 1.1 mmol, 1.1 eq.) and the mixture stirred at reflux for 4 hours. The reaction mixture was then concentrated in vacuo and partitioned between saturated NaHCO3 solution (20 mL) and DCM (2×20 mL). The organics were combined, dried over sodium sulphate, filtered and concentrated in vacuo to give the title compound (475 mg, 100%) as a yellow oil. LRMS APCI+ m/z 441 [MH]+.

1. temperatureat reflux for 4 hours
2. concentrationThe reaction mixture was then concentrated in vacuo
3. custompartitioned between saturated NaHCO3 solution (20 mL) and DCM (2×20 mL)
4. dry with materialdried over sodium sulphate
5. filtrationfiltered
6. concentrationconcentrated in vacuo