7139-02-8

Beige Solid

An antitumor nucleoside pyrimido pyrimidine.

General procedure for the synthesis of 2,6-dichloro-4,8-dipiperidinosubstituted pyrimido[5,4-d]pyrimidines from hexahydropyridine and perchloropyrimido[5,4-d]pyrimidines: perchloropyrimido[5,4-d]pyrimidines (13.1 g, 48.9 mmol), piperidines, CuI (0.28 g, 1.5 mmol) and Cs2CO3 (16.0 g, 48.9 mmol) were added to a 250mL two-necked flask. 100 mL of nitrobenzene was added as reaction solvent and the reaction was carried out at 180°C for 16 h under nitrogen protection. After completion of the reaction, the nitrobenzene solvent was removed by distillation under reduced pressure. Purification by column chromatography using a solvent mixture of petroleum ether (PE) and dichloromethane (DCM) (6:1, v/v) gave 17.0 g of solid product in 95.0% yield and 99% selectivity.

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