反应详情

温度

35 °C

The product of Example 93, Step 5 (75 mg, 0.168 mmol, 1.0 equiv) was cooled to −78° C. in 1.75 mL CH2Cl2 and BCl3 (1.0 M in CH2Cl2, 2.5 mL, 2.526 mmol, 15.0 equiv) was added dropwise. The reaction was warmed to 35° C. and stirred for 90 hours. An additional portion of BCl3 (2.5 mL, 2.526 mmol, 15.0 equiv) in CH2Cl2 was added dropwise and the reaction was stirred for another 96 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 (10-90% CH3CN/H2O, 0.1% TFA over 18 minutes, retention time 10.55 min) to provide 16 mg (22%) of the title compound as a white solid. MS (ES+) m/e 432 [M+H]+

1. stirringthe reaction was stirred for another 96 hours
2. customThe phases were separated
3. filtrationThe precipitate was filtered
4. washwashed with Et2O
5. customThe residue was purified by reverse-phase HPLC (10-90% CH3CN/H2O, 0.1% TFA over 18 minutes, retention time 10.55 min)