反应详情

1.39 ml (8.40 mmol) of diisopropylethylamine are added to a suspension of 0.840 g (7 mmol) of 1H-[1,2,3]triazolo[4,5-b]pyridine, of 1.741 g (7 mmol) of tert-butyl 4-chlorocarbonylpiperazine-1-carboxylate (Bioorg. Med. Chem. Lett. 2000, 10, 2357) and of 0.042 g (0.35 mmol) of 4-dimethylaminopyridine in 14 ml of tetrahydrofuran. The mixture is stirred at ambient temperature for 4 hours and then 80 ml of ethyl acetate and 20 ml of water are added. The organic phase is separated by settling out and is then washed with 3×20 ml of water and 20 ml of a saturated aqueous solution of sodium chloride. The product is dried over sodium sulfate and evaporated to dryness. The residue is recrystallized from isopropanol, so as to obtain 1.70 g (5.1 mmol) of product in the form of white crystals.

1. customThe organic phase is separated
2. washis then washed with 3×20 ml of water and 20 ml of a saturated aqueous solution of sodium chloride
3. dry with materialThe product is dried over sodium sulfate
4. customevaporated to dryness
5. customThe residue is recrystallized from isopropanol