反应详情

The intermediate dihydrophenanthridine was prepared from 6-ethyl-8-fluorophenanthridine (1.10 g, 4.88 mmol) by treatment with sodium borohydride (1.11 g, 29.3 mmol) and trifluoroacetic acid (1.50 mL, 19.5 mmol) in tetrahydrofuran (18 mL). In a separate, second step, the dihydrophenanthridine was treated with triethylamine (4.1 mL, 29.3 mmol) and 4-methoxybenzenesulfonyl chloride (1.11 g, 5.37 mmol) in dichloromethane (5 mL) according to the procedure and in the same manner as described in Example 32, Method A, Step d. The crude product was purified by flash column chromatography on silica gel, eluting with a mixture of ethyl acetate-hexane (1:9 to 3:7 gradient), to yield 6-ethyl-8-fluoro-5-[(4-methoxyphenyl)sulfonyl]-5,6-dihydrophenanthridine as a homogeneous, white, crystalline, solid (1.67 g, 87%), m.p. 153-156° C.;

1. customThe crude product was purified by flash column chromatography on silica gel
2. washeluting with a mixture of ethyl acetate-hexane (1:9 to 3:7 gradient)