反应详情

温度

10 °C

A solution of 3.86 g (14.23 mmol) of trans-4-[(tert-butoxycarbonyl-methyl-amino)-methyl]-cyclohexanecarboxylic acid was dissolved in 36 mL of dioxane, cooled to 10° C. and treated with 35.5 mL (142.25 mmol, 10 eq) of 4M HCl in dioxane, then warmed to RT. The solution was evaporated after 2 h 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 2.66 g (90%) of trans-4-methylaminomethyl-cyclohexanecarboxylic acid·HCl, MS: 172 (MH+), MP: 261° C.

1. temperaturewarmed to RT
2. customThe solution was evaporated after 2 h 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