反应详情

温度

35 °C

The product from Example 95 (105 mg, 0.247 mmol, 1.00 equiv) was cooled to −78° C. in 2.0 mL CH2Cl2 and BCl3 (1.0 M in CH2Cl2, 3.70 mL, 3.71 mmol, 15.0 equiv) was added dropwise. The reaction was warmed to 35° C. and stirred for 90 hours. The reaction mixture was diluted with EtOAc and water and basified to pH 14 with 6N NaOH. The phases were separated, and the aqueous phase was acidified to pH 4 with 6N HCl. The precipitate was filtered and washed with Et2O. The residue was purified by reverse-phase HPLC (10-95% CH3CN/H2O, 0.1% TFA over 18 minutes, retention time 9.15 min) to provide 20 mg (20%) of the title compound as a white solid. MS (ES+) m/e 411 [M+H]+

1. customThe phases were separated
2. filtrationThe precipitate was filtered
3. washwashed with Et2O
4. customThe residue was purified by reverse-phase HPLC (10-95% CH3CN/H2O, 0.1% TFA over 18 minutes, retention time 9.15 min)