反应详情

Under argon, 100 mg (0.44 mmol) of the compound of Example 2A, 57.97 mg (0.44 mmol) 4-formylbenzonitrile and 49.57 mg (0.44 mmol) 2-cyano-N,N-dimethylacetamide are dissolved in 2 ml ethanol. 3.76 mg (4.4 μl, 0.04 mmol) piperidine are added, and the mixture is stirred at reflux overnight. After cooling down to room temperature, the crude product is purified by column chromatography with cyclohexane/ethyl acetate 20:1, 10:1, 8:1, 6:1, 4:1, 2:1, 1:1, 1:2 and dichloromethane/methanol 100:1, 50:1, 20:1 as eluents. The product containing fractions are repurified by preparative HPLC.

1. temperatureat reflux overnight
2. customthe crude product is purified by column chromatography with cyclohexane/ethyl acetate 20:1, 10:1, 8:1, 6:1, 4:1, 2:1, 1:1, 1:2 and dichloromethane/methanol 100:1, 50:1, 20:1 as eluents
3. additionThe product containing fractions
4. customare repurified by preparative HPLC