反应详情

To 33.5 mg (120 μmol) 2-[4-(4-ethoxy-phenylethynyl)-phenyl]-1-methyl-ethylamine (I64) in 2.0 mL ACN are added 166 mg (1.20 mmol) K2CO3, a few crystals DMAP and finally 23.5 μL (0.18 mmol) 3-chloropivaloyl chloride (in 1.0 mL ACN). The reaction mixture is stirred at reflux for 6 h. The solvent is removed in vacuo and the residue is resolved EtOAc and washed with water (1×), sat. aq. NaHCO3 solution (2×) and again with water. The organic layer is dried with Na2SO4 and the solvent is evaporated in vacuo. The residue is purified by HPLC (MeOH/H2O/TFA).

1. temperatureat reflux for 6 h
2. customThe solvent is removed in vacuo
3. washwashed with water (1×), sat. aq. NaHCO3 solution (2×) and again with water
4. dry with materialThe organic layer is dried with Na2SO4
5. customthe solvent is evaporated in vacuo
6. customThe residue is purified by HPLC (MeOH/H2O/TFA)