反应详情

温度

30 °C

The product from Example 96 (0.050 g, 0.11 mmol, 1.0 equiv) was cooled to −78° C. in 1.5 mL CH2Cl2 and BCl3 (1.0 M in CH2C2, 1.70 mL, 1.71 mmol, 15.0 equiv) was added dropwise. The reaction was warmed to 30° C. and stirred for 72 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 and the product was extracted into EtOAc. The organic layer was washed with sat'd NaCl and concentrated en vacuo. The residue purified by reverse-phase HPLC (10-95% CH3CN/H2O, 0.1% TFA over 6 minutes, retention time 3.48 min) to provide 1 mg (0.7%) of the title compound as a white solid. MS (ES+) m/e 425 [M+H]+

1. customThe phases were separated
2. extractionthe product was extracted into EtOAc
3. washThe organic layer was washed with sat'd NaCl
4. concentrationconcentrated en vacuo
5. customThe residue purified by reverse-phase HPLC (10-95% CH3CN/H2O, 0.1% TFA over 6 minutes, retention time 3.48 min)