反应详情

A mixture of sulfone 9.1 (1.0 g, 2.4 mmol), diphenyl-2-pyridylphosphine (1.9 g, 7.23 mmol) and 4-hydroxy-1-methylpiperidine (0.555 g, 4.8 mmol) was dissolved in anhydrous tetrahydrofuran under an atmosphere of nitrogen. To this solution was added di-tert-butylazodicarboxylate (1.67 g, 7.23 mmol) and the resulting mixture was stirred at room temperature for 2 hours, then concentrated in vacuo. The residue was purified by column chromatography on silica gel using 9:1 dichloromethane/methanol as eluant. The column fractions containing product were combined and concentrated in vacuo to give 354 mg of 7-benzylsulfonyl-3-(2-chlorophenyl)-1-(1-methylpiperidin-4-yl)-3,4-dihydropyrimido[4,5-d]pyrimidin-2(1H)-one.

1. concentrationconcentrated in vacuo
2. customThe residue was purified by column chromatography on silica gel using 9:1 dichloromethane/methanol as eluant
3. additionThe column fractions containing product
4. concentrationconcentrated in vacuo