反应详情

Methyl 6-chloro-5-nitronicotinate (2 g, 9.23 mmol) was added to ethyl 2-(isopropylamino)acetate (5.0 g, 34.5 mmol) neat while stirring at room temperature. The viscous yellow reaction was heated to 90° C. for one h and then allowed to cool back to room temperature. The reaction was diluted with dichloromethane (20 mL) and purified via column chromatography (220 g SiO2, 20-30% gradient, ethyl acetate in hexanes) to yield the title compound (2.39 g, 83%) as a yellow oil. [M+H] calc'd for C, 14; H, 19; N, 3; O, 6, 326; found, 326.

1. customThe viscous yellow reaction
2. temperaturewas heated to 90° C. for one h
3. temperatureto cool back to room temperature
4. custompurified via column chromatography (220 g SiO2, 20-30% gradient, ethyl acetate in hexanes)