反应详情

温度

80 °C

A stirred mixture of 4-aminomethyl-4-hydroxy-piperidine-1-carboxylic acid tert-butyl ester (529 mg, 2.3 mmol) in tetrahydrofuran (15 ml) was added slowly with lithium aluminum hydride (0.88 g, 23 mmol) while maintaining the temperature at 0˜5° C. Upon completion of the addition, the mixture was stirred at 80° C. in oil bath overnight. The mixture was added with potassium sodium tartrate tetrahydrate (6.3 g, 22.3 mmol) and stirred for 8 hours at room temperature. The mixture was filtered and washed with tetrahydrofuran (10 ml×3). The combined organic extracts were concentrated under reduced pressure to give 4-aminomethyl-1-methyl-piperidin-4-ol (245 mg, 74%) as a white oil which was used as such.

1. temperaturewhile maintaining the temperature at 0˜5° C
2. additionUpon completion of the addition
3. stirringstirred for 8 hours at room temperature
4. filtrationThe mixture was filtered
5. washwashed with tetrahydrofuran (10 ml×3)
6. concentrationThe combined organic extracts were concentrated under reduced pressure