甲基[2-甲基-1-(吡咯烷-1-基)丙-2-基]胺

反应条件: temp:40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of tert-butyl 2-methyl-1-oxo-1-(pyrrolidin-1-yl)propan-2-ylcarbamate (Compound F5) (2.696 g, 10.52 mmol) in THF (20 mL) was a 1M LAH in THF (42.1 mL, 42.07 mmol) solution dropwise added (over approximately 10 min) at 0° C. under a nitrogen atmosphere. The resultant mixture was stirred at rt for 1 h and heated at 40° C. over night. The reaction was cooled to 0° C. and Na2SO4×10H2O followed by NaOH (2M, 2 mL) was added. The mixture was diluted with Et2O (100 mL) and the resultant mixture was filtered. The solids were washed with Et2O (3×50 mL). To the filtrate was HCl (1.25 N aq. solution, 15 mL) in EtOH added. The filtrate was concentrated and the residue mixed with EtOH (60 mL). The EtOH was removed under reduced pressure. IPA (30 mL) was added and the mixture sonicated for 2 min. After filtration was the title compound (1.89 g, 96%) obtained as a HCl salt. 1H NMR (400 MHz, CDCl3) δ 1.00, 1.71, 2.29, 2.41, 2.63. Total no of protons: 19. dropwise added (over approximately 10 min) at 0° C. under a nitrogen atmosphere The reaction was cooled to 0° C. was added the resultant mixture was filtered The solids were washed with Et2O (3×50 mL) added The filtrate was concentrated the residue mixed with EtOH (60 mL) The EtOH was removed under reduced pressure IPA (30 mL) was added the mixture sonicated for 2 min After filtration