反应详情

温度

100 °C

A mixture of 2.97 g (8.0 mmol) 5-bromo-2-[4-(2-pyrrolidin-1-yl-ethoxy)-phenylethynyl]-pyridine, 2.50 g (16.0 mmol) 4-chloro-phenylboric acid, 462 mg (0.4 mmol) tetrakis-triphenylphosphane-palladium and 8.0 mL of a 2M aqueous Na2CO3 solution in 100 mL 1,4-dioxane is heated for 4 h at 100° C. under an argon atmosphere. The solvent is distilled off i.vac., the residue is stirred with water/EtOAc (1/1, v/v), suction filtered through a fibreglass filter, the organic phase is washed with saturated, aqueous NaCl solution and dried over Na2SO4. After the desiccant and solvent have been eliminated the residue is purified by chromatography (Alox, cyc/EtOAc 2:1). The product fractions are evaporated down, the residue is triturated with diethyl ether, suction filtered and washed with diethyl ether.

1. distillationThe solvent is distilled off i.vac
2. filtrationv/v), suction filtered through a fibreglass
3. filtrationfilter
4. washthe organic phase is washed with saturated, aqueous NaCl solution
5. dry with materialdried over Na2SO4
6. customis purified by chromatography (Alox, cyc/EtOAc 2:1)
7. customThe product fractions are evaporated down
8. customthe residue is triturated with diethyl ether, suction
9. filtrationfiltered
10. washwashed with diethyl ether