反应详情

1-(Amino)-2-(vinyl)cyclopropanecarboxylic acid ethyl ester hydrochloride (4.92 g, 31.7 mmol) and HATU (12.6 g, 33.2 mmol) were added to the acid (142) (8.14 g, 30.2 mmol). The mixture was cooled in an ice bath under argon, and then DMF (100 mL) and DIPEA (12.5 mL, 11.5 mmol) were added. After 30 min at 0° C., the solution was stirred at room temperature for an additional 3 h. Then, the reaction mixture was partitioned between EtOAc and water, washed successively with 0.5 N HCl (20 mL) and saturated NaCl (2×20 mL), and dried (Na2SO4). Purification by flash chromatography (EtOAc/CH2Cl2/Petroleum ether, 1:1:1) afforded the title compound (7.41, g 60%) as a colorless oil, m/z=407 (M+H)+.

1. temperatureThe mixture was cooled in an ice bath under argon
2. customThen, the reaction mixture was partitioned between EtOAc and water
3. washwashed successively with 0.5 N HCl (20 mL) and saturated NaCl (2×20 mL)
4. dry with materialdried (Na2SO4)
5. customPurification by flash chromatography (EtOAc/CH2Cl2/Petroleum ether, 1:1:1)