反应详情

温度

65 °C

A solution of methanesulfonic acid 1,4-dioxa-spiro[4.5]dec-8-yl ester (567 mg, 2.40 mmol) and 1,2,4-triazole (232 mg, 3.36 mmol) in dry DMF (5.00 mL) was treated with sodium hydride 60% (125 mg, 3.12 mmol) at room temperature under nitrogen. The resulting mixture was stirred at 65° C. for 72 h. It was poured in ice water (75 mL), extracted 3 portions of 75 mL of EtOAc. The organic portions were combined, dried over anhydrous Na2SO4 and concentrated. The solid was purified by silica gel column chromatography using a gradient from 100% EtOAc to 5% MeOH:EtOAc as eluent to furnished the final compound 1-(1,4-dioxa-spiro[4.5]dec-8-yl)-1H-[1,2,4]triazole as a white solid (247 mg, 49%).

1. extractionextracted 3 portions of 75 mL of EtOAc
2. dry with materialdried over anhydrous Na2SO4
3. concentrationconcentrated
4. customThe solid was purified by silica gel column chromatography