反应详情

To a solution of crude 5-amino-5-(2-methoxyphenyl)-1-pentene (1.63 g) in CH2Cl2 (10 mL) at 0° C. was added DMAP (1.15 g, 9.38 mmol) followed by Cbz-Cl (1.34 mL, 9.38 mmol) and the resulting solution was stirred at room temperature overnight. Ether was added, the aqueous layer was extracted with diethyl ether (x4), and the combined organic layers was washed with brine, dried over MgSO4 and evaporated in vacuo. The crude product was purified by silica gel flash chromatography (5% EtOAc-95% hexanes) to provide the title compound as a white solid (1.84 g). 1H NMR (CDCl3, 400 MHz) δ: 3.82 (3H, s, OMe), 2.0 (4H, m).

1. extractionthe aqueous layer was extracted with diethyl ether (x4)
2. washthe combined organic layers was washed with brine
3. dry with materialdried over MgSO4
4. customevaporated in vacuo
5. customThe crude product was purified by silica gel flash chromatography (5% EtOAc-95% hexanes)