反应详情

Oxalyl chloride (0.06 ml, 0.69 mmol) was added to a solution of 3-Methyl-isoxazole-4-carboxylic acid (0.06 g, 0.48 mmol) followed by 1 drop of dimethylformamide. The mixture was stirred at room temperature for 4 hours before concentrating in vacuo and azeotroping with dichloromethane. The residue was taken up in pyridine (1 ml) and added to a solution of 3-chloro-pyrazine-2,6-diamine (Preparation 1) (0.035 g, 0.24 mmol) in anhydrous pyridine (3 ml) and the mixture heated at 50° C. for 3 hours before cooling to room temperature and concentrating to dryness in vacuo. The residue was purified by silica gel column chromatography, eluting with ethyl acetate:heptane 1:1, to afford the product as a white solid (30 mg).

1. concentrationbefore concentrating in vacuo
2. customazeotroping with dichloromethane
3. temperaturethe mixture heated at 50° C. for 3 hours
4. temperaturebefore cooling to room temperature
5. concentrationconcentrating to dryness in vacuo
6. customThe residue was purified by silica gel column chromatography
7. washeluting with ethyl acetate:heptane 1:1