反应详情

温度

0 °C

An ice-cold solution of 1,4-dioxaspiro[4,5]-decane-8-acetic acid (20.0 g) (Example G) and triethylamine (20.9 ml) in 100 ml of dichloromethane is treated dropwise with a solution of isobutyl chloroformate (19.4 ml) in 100 ml of dichloromethane under nitrogen. The resulting solution is stirred at 0° C. for 10 minutes and a solution of 1-(2-pyridyl)-piperazine (32.59 g) in 100 ml of dichloromethane is added dropwise. The mixture is stirred at 0° C. for 15 minutes and then at room temperature for one hour. After washing with 1 L of a saturated solution of sodium bicarbonate, the organic phase is dried over magnesium sulfate and concentrated in vacuo. The crude product is purified by MPLC (silica; ethyl acetate) to give 25.50 g of the title compound as a colorless solid; mp 113°-116° C.

1. stirringThe mixture is stirred at 0° C. for 15 minutes
2. waitat room temperature for one hour
3. washAfter washing with 1 L of a saturated solution of sodium bicarbonate
4. dry with materialthe organic phase is dried over magnesium sulfate
5. concentrationconcentrated in vacuo
6. customThe crude product is purified by MPLC (silica; ethyl acetate)