反应详情

To a mixture of 1-bromo-3-nitrobenzene (300 mg, 1.48 mmol), 2-(methoxymethyl)pyrrolidine (187 mg, 1.63 mmol), Cs2CO3 (800 mg, 2.45 mmol), X-Phos (50 mg, 0.1 mmol), Pd(dba)2 (50 mg, 0.087 mmol) in 50 mL of dioxane were stirred at reflux overnight under N2 atmosphere. The excess of dioxane was removed under reduced pressure and the residue was purified by silica gel chromatography, eluting with a mixture of petroleum ether and ethyl acetate (5:1) to give 2-(methoxymethyl)-1-(3-nitrophenyl)pyrrolidine (250 mg, 72%) as a yellow solid. LC-MS: 237 [M+H]+, tR=1.71 min.

1. temperatureat reflux overnight under N2 atmosphere
2. customThe excess of dioxane was removed under reduced pressure
3. customthe residue was purified by silica gel chromatography
4. washeluting with a mixture of petroleum ether and ethyl acetate (5:1)