反应详情

To a solution of tert-butyl N-(2-{[5-(trifluoromethyl)pyridin-2-yl]methyl}cyclopentyl)carbamate (1.0 g, 2.9 mmol) in 1,4-dioxane (5 ml) at 0° C. was added drop wise HCl in 1,4-dioxane (12%, 15.0 ml). The reaction was stirred at room temperature for 1 hour, then concentrated in vacuo. To this was then added DCM (50 ml) and a solution of sodium bicarbonate (aq, 7.5%, 15 ml). The organics were dried over sodium sulfate and concentrated in vacuo. The resulting residue was purified by column chromatography (0-2% methanol/DCM) and then treated with HCl in 1,4-dioxane (12%, 5 ml), stirred for 2 hours, concentrated in vacuo, triturated with diethyl ether to afford the title compound as a single diastereomer.

1. concentrationconcentrated in vacuo
2. dry with materialThe organics were dried over sodium sulfate
3. concentrationconcentrated in vacuo
4. customThe resulting residue was purified by column chromatography (0-2% methanol/DCM)
5. additiontreated with HCl in 1,4-dioxane (12%, 5 ml)
6. stirringstirred for 2 hours
7. concentrationconcentrated in vacuo
8. customtriturated with diethyl ether