反应详情

A solution of 2,6-dichloro-5-nitropyridine (46) (0.5 g) in THE (20 mL) was cooled to 0° C. and treated with 1.6 mL triethylamine followed by (R)-1-pyridin-3-yl-ethylamine (300 μL). The mixture was stirred for 1.5 h, then warmed to RT and stirred another 20 h. 2,4-Dimethoxybenzylamine (0.8 mL) was added and the mixture was heated at 50° C. for four hours. The mixture was diluted with ethyl acetate and washed twice with saturated sodium chloride solution. The organic layer was separated, dried over sodium sulfate, filtered, and concentrated. Column chromatography (50→100% ethyl acetate in hexanes) provided 761 mg of (R)—N6-(2,4-Dimethoxybenzyl)-3-nitro-N2-(1-(pyridin-3-yl)ethyl)pyridine-2,6-diamine (64).

1. stirringstirred another 20 h
2. temperaturethe mixture was heated at 50° C. for four hours
3. washwashed twice with saturated sodium chloride solution
4. customThe organic layer was separated
5. dry with materialdried over sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated