反应详情

温度

90 °C

2-Chloro-4-nitro-pyridine (476 mg, 3 mmol), cyclopropanecarboxylic acid amide (306 mg, 3.6 mmol), and tripotassium phosphate (892 mg, 4.2 mmol) are mixed in dimethoxyethane under an argon atmosphere. (2′-Dicyclohexylphosphanyl-biphenyl-2-yl)-dimethyl-amine (118 mg, 0.3 mmol) and Pd2(dba)3 (275 mg, 0.3 mmol) are added and the mixture is stirred for 3 h at 90° C. Further 0.5 equivalent cyclopropanecarboxylic acid amide (128 mg, 1.5 mmol) is added and the mixture is stirred for 1 additional hour. After cooling at RT the reaction mixture is taken in ethyl acetate, washed with a solution of saturated sodium hydrogen carbonate and brine. The combined organic phases are dried (Na2SO4), concentrated under reduced pressure and the residue is purified by column chromatography (ethyl acetate/hexane) to afford the title compound as a brown solid. M-H−=206.1, HPLC tR: 4.62 min.

1. stirringthe mixture is stirred for 1 additional hour
2. temperatureAfter cooling at RT the reaction mixture
3. washwashed with a solution of saturated sodium hydrogen carbonate and brine
4. dry with materialThe combined organic phases are dried (Na2SO4)
5. concentrationconcentrated under reduced pressure
6. customthe residue is purified by column chromatography (ethyl acetate/hexane)