反应详情

A mixture of compound 3-e (1.6 g, 6.9 mmol), 2,2-diphenylacetic acid (1.47 g, 6.9 mmol), DIEA (1.8 g, 13.8 mmol), and TBTU (2.7 g, 8.28 mmol) in DMF (20 mL) was stirred at room temperature overnight. The reaction mixture was added with sat. NH4Cl (50 mL), extracted with DCM (100 mL), washed with water (50 mL) and brine ((50 mL). The organic layer was concentrated and purified by column chromatography to afford the product as a white solid, 3-f (2.2 g, 76%). 1H NMR (300 MHz, CDCl3) δ 4.45 (s, 2H), 4.63 (s, 2H), 5.07 (s, 1H), 7.27-7.40 (m, 16H), LC-MS (M+H)+ 426.1

1. extractionextracted with DCM (100 mL)
2. washwashed with water (50 mL) and brine ((50 mL)
3. concentrationThe organic layer was concentrated
4. custompurified by column chromatography