反应详情

温度

90 °C

To a solution of Intermediate 14A (0.88 g, 3.64 mmol) in DMF (10 mL) was added tert-butyl acrylate (1.401 g, 10.93 mmol), TEA (1.270 mL, 9.11 mmol) and Pd(OAc)2 (0.082 g, 0.364 mmol). The reaction was warmed to 90° C. After 5 h, the reaction was cooled to rt and then filtered to remove the solid. The filtrate was diluted with EtOAc, washed with 1M HCl, saturated NaHCO3, and brine. The organic phase was dried over MgSO4, filtered and concentrated. Purification by normal phase chromatography gave Intermediate 14B (232 mg, 22% yield) as a tan oil. MS (ESI) m/z: 233.1 (M-tBu)+.

1. temperaturethe reaction was cooled to rt
2. filtrationfiltered
3. customto remove the solid
4. additionThe filtrate was diluted with EtOAc
5. washwashed with 1M HCl, saturated NaHCO3, and brine
6. dry with materialThe organic phase was dried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated
9. customPurification by normal phase chromatography