反应详情

温度

0 °C

To a 0° C. solution of 400 mg (2.12 mmol) (5-methyl-pyridin-2-yl)-acetic acid hydrochloride (CAS: 848093-05-0) in 7.5 mL dichloromethane were added successively 250 mg (2.02 mmol) 3,4-dimethylaniline and 415.4 mg (2.12 mmol) 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride. The mixture was stirred at 0° C. for 45 minutes. The solution was washed with a sat. NaHCO3 solution, NaOH 2N and with water, dried over Na2SO4, filtered and concentrated in vacuo. The crude solid was purified with flash column chromatography on silica eluting with a gradient formed from heptane and ethylacetate to provide 0.40 g (77%) of the title compound as an off-white solid. MS (m/e): 255.2 [M+H]+.

1. washThe solution was washed with a sat. NaHCO3 solution, NaOH 2N and with water
2. dry with materialdried over Na2SO4
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. customThe crude solid was purified with flash column chromatography on silica eluting with a gradient
6. customformed from heptane and ethylacetate