反应详情

2-Amino-4,4-dimethyl-pentanoic acid methyl ester (5.35 g, 27.4 mmol) was dissolved in 100 mL of dichloromethane. Hunig's base (7.07 g, 54.7 mmol) and 4-morpholinecarbonyl chloride (4.08 g, 27.4 mmol) were added and the reaction was stirred at ambient temperature 16 h. The reaction mixture was concentrated in vacuo and taken up in 150 mL EtOAc. A white precipitate formed and was filtered and washed with EtOAc. EtOAc solutions were combined and washed with 3×50 mL 1 N HCl (aq), 3×50 saturated NaHCO3 (aq), and 1×50 mL brine. The organic layer was dried over Na2SO4, decanted, and concentrated to a white solid (6.33 g). MS, m/z 273=M+1.

1. concentrationThe reaction mixture was concentrated in vacuo
2. customA white precipitate formed
3. filtrationwas filtered
4. washwashed with EtOAc
5. washwashed with 3×50 mL 1 N HCl (aq), 3×50 saturated NaHCO3 (aq), and 1×50 mL brine
6. dry with materialThe organic layer was dried over Na2SO4
7. customdecanted
8. concentrationconcentrated to a white solid (6.33 g)