反应详情

To a solution of t-butylglycine (1.40 g, 10.67 mmol) in acetonitrile (20 mL) cooled to 0° C. was added ethyldisopropylamine (1.86 mL, 10.67 mmol) and t-butyl bromoacetate (1.57 mL, 10.67 mmol). The resulting solution was stirred for 24 h at room temperature. The mixture was concentrated to dryness in vacuo, water was added and the solution was extracted with dichloromethane (3×70 mL). The combined organic phases were washed with brine (70 mL), dried over Na2SO4 and concentrated to dryness in vacuo. The crude material was purified by silica gel chromatography (20-80% EtOAc in hexanes) to give the compound 14 (0.88 g, 33.6%). 1H NMR (400 MHz, CDCl3) δ 1.43 (s, 18H), 3.30 (s, 4H).

1. concentrationThe mixture was concentrated to dryness in vacuo, water
2. additionwas added
3. extractionthe solution was extracted with dichloromethane (3×70 mL)
4. washThe combined organic phases were washed with brine (70 mL)
5. dry with materialdried over Na2SO4
6. concentrationconcentrated to dryness in vacuo
7. customThe crude material was purified by silica gel chromatography (20-80% EtOAc in hexanes)