反应详情

To a solution of methyl 1-(methylamino)cyclopropanecarboxylate (1.53 g, 11.85 mmol) and HOBt (1.920 g, 14.21 mmol) in CH2Cl2 (30 mL) was added 4-methylmorpholine (5.2 mL, 47.40 mmol), N-{[(phenylmethyl)oxy]carbonyl}glycine (2.48 g, 11.85 mmol), and EDCI (2.73 g, 14.21 mmol). After stirring overnight, the solution was washed 6 N aq. HCl (100 mL) and water (100 mL). The aqueous layers were extracted with CH2Cl2 (1×100 mL), and the combined organic layers were washed with water (100 mL) and brine (100 mL), then dried over anhydrous MgSO4 and concentrated in vacuo to provide pure methyl 1-[methyl(N-{[(phenylmethyl)oxy]carbonyl}glycyl)amino]cyclopropanecarboxylate (3.66 g, 97%). LCMS: (M+H)+: 321.1.

1. washthe solution was washed 6 N aq. HCl (100 mL) and water (100 mL)
2. extractionThe aqueous layers were extracted with CH2Cl2 (1×100 mL)
3. washthe combined organic layers were washed with water (100 mL) and brine (100 mL)
4. dry with materialdried over anhydrous MgSO4
5. concentrationconcentrated in vacuo