反应详情

温度

10 °C

A solution of 5.15 g (20.0 mmol) of trans-4-(tert-butoxycarbonyl-methyl-amino)-cyclohexanecarboxylic acid was dissolved in 50 mL of dioxane, cooled to 10° C. and treated with 50 mL (200 mmol, 10 eq) of 4M HCl in dioxane, then warmed to RT overnight. The solution was evaporated to ca. 15 mL, cooled to 0° C. and precipitated with ˜100 mL of Et2O. The solid precipitate was filtrated, washed with Et2O (×3) and dried under reduced pressure to yield 3.76 g (97%) of trans-4-methylamino-cyclohexanecarboxylic acid-HCl, MS: 156 (M−H−), MP: 249° C., dec.

1. temperaturewarmed to RT overnight
2. customThe solution was evaporated to ca. 15 mL
3. temperaturecooled to 0° C.
4. customprecipitated with ˜100 mL of Et2O
5. filtrationThe solid precipitate was filtrated
6. washwashed with Et2O (×3)
7. customdried under reduced pressure