反应详情

温度

110 °C

A mixture of 200 mg (0.54 mmol) {2-[4-(5-bromo-pyridin-2-ylethynyl)-phenoxy]-ethyl}-diethyl-amine, 163 mg (1.07 mmol) 4-methoxy-phenylboric acid, 31 mg (0.03 mmol) tetrakis-triphenylphosphane-palladium and 0.27 mL of a 2 M aqueous Na2CO3 solution in 5 mL 1,4-dioxane is heated for 20 h at 110° C. under a nitrogen atmosphere. The solvent is distilled off i.vac., the residue is taken up in water, exhaustively extracted with EtOAc and dried over Na2SO4. After the desiccant and solvent have been eliminated the residue is purified on silica gel (EtOAc/MeOH/NH3 95:5:0.5). The product fractions are evaporated down, the residue is triturated with diethyl ether, suction filtered and washed with diisopropylether.

1. distillationThe solvent is distilled off i.vac
2. extractionexhaustively extracted with EtOAc
3. dry with materialdried over Na2SO4
4. customis purified on silica gel (EtOAc/MeOH/NH3 95:5:0.5)
5. customThe product fractions are evaporated down
6. customthe residue is triturated with diethyl ether, suction
7. filtrationfiltered
8. washwashed with diisopropylether