反应详情

Dissolve 7,9-difluoro-5-[4-(2-piperidin-1-yl-ethoxy)-phenyl]-5H-6-oxa-chrysen-2-ol (1.6 g, 3.3 mmol) in methylene chloride (20 mL). Add 2M HCl in ether (3.3 mL, 6.6 mmol) and concentrate in vacuo. Dissolve the residue in methylene chloride (5 mL) and add dropwise to vigorously stirred ether (30 mL). Filter the precipitate and dry in a 50° C. vacuum oven overnight to obtain 1.5 g (87%) of the title compound. Mass spectrum (ion spray): m/z=488.3 (M+H−HCl).

1. concentrationconcentrate in vacuo
2. dissolutionDissolve the residue in methylene chloride (5 mL)
3. additionadd dropwise to vigorously stirred ether (30 mL)
4. filtrationFilter the precipitate
5. customdry in a 50° C. vacuum oven overnight