反应详情

温度

0 °C

A solution of trans-acetamide 4 (9.0 g, 26.9 mmol), n-propanol (45 mL) and 5M hydrochloric acid (45 mL) was refluxed for approximately 48 h (90-93° C.). During this time, the reaction temperature was maintained at ≧90° C. by periodically collecting the distillate until the reaction temperature was >92° C. Additional n-propanol was added periodically to maintain the solution at its original volume. After the hydrolysis was complete, the solution was slowly cooled to 0° C., resulting in a slurry, which was aged for one hour at 0° C. The reaction mixture was filtered, and the cake was washed with 1:1 methanol/water (20 mL), followed by t-butyl methyl ether (20 mL). The wet-cake was dried under vacuum at 45 to 50° C. to afford 7.0 g of the amine hydrochloride 5 (80% yield).

1. temperatureDuring this time, the reaction temperature was maintained at ≧90° C.
2. distillationby periodically collecting the distillate until the reaction temperature
3. customwas >92° C
4. additionAdditional n-propanol was added periodically
5. temperatureto maintain the solution at its original volume
6. customresulting in a slurry, which
7. filtrationThe reaction mixture was filtered
8. washthe cake was washed with 1:1 methanol/water (20 mL)
9. customThe wet-cake was dried under vacuum at 45 to 50° C.