反应详情

温度

70 °C

A 250-mL round-bottomed flask was charged with di-tert-butyl (2S)-2-(((3S)-3-methyl-4-morpholinyl)methyl)-1,4-piperazinedicarboxylate (2.46 g, 6.16 mmol, step 2), HCl (4.0 M solution in 1,4-dioxane, 4.62 mL, 18.5 mmol, Sigma-Aldrich, St. Louis, Mo.) and EtOAc (100 mL). The reaction mixture was heated at 70° C. for 3 h. At this time, additional HCl (4.0 M solution in 1,4-dioxane, 5.00 mL, 20.0 mmol) was added and heating at 70° C. was resumed for an additional 3 h. The reaction mixture was cooled to room temperature and the resulting white solid was collected, washed with EtOAc and dried overnight under reduced pressure to afford (3S)-3-methyl-4-((2R)-2-piperazinylmethyl)morpholine trihydrochloride (2.05 g) as a white powder.

1. temperatureheating at 70° C.
2. temperatureThe reaction mixture was cooled to room temperature
3. customthe resulting white solid was collected
4. washwashed with EtOAc
5. customdried overnight under reduced pressure