反应详情

HATU (16.25 g, 42.7 mmol) was added to a stirred solution of 4-iodobenzene-1,2-diamine (10 g, 42.7 mmol), (S)-2-((tert-butoxycarbonyl)amino)-3,3-dimethylbutanoic acid (9.88 g, 42.7 mmol) and DIPEA (14.93 mL, 85 mmol) in DMF (120 mL) at 0° C. and the reaction mixture was stirred at rt for 12 h. The reaction mixture was diluted with water and EtOAc. The organic layer was washed with water, 10% NaHCO3 solution, brine, dried over Na2SO4 and concentrated to yield (S)-tert-butyl (1-((2-amino-5-iodophenyl)amino)-3,3-dimethyl-1-oxobutan-2-yl)carbamate (20 g). LC/MS (Condition B-10): Rt=1.94 min. LC/MS: Anal. Calcd. for [M+H]+ C17H27IN3O3: 448.10; found 448.2.

1. washThe organic layer was washed with water, 10% NaHCO3 solution, brine
2. dry with materialdried over Na2SO4
3. concentrationconcentrated