反应详情

温度

180 °C

A mixture of 8-methoxy-11-methyl-6,11-dihydro-5-thia-4,11-diaza-benzo[a]fluorene (100 mg, 0.355 mmoL) and pyridine HCl salt (410 mg, 3.55 mmoL) was sealed in a tube and heated to 180° C. for 2 hours. The reaction mixture was cooled and the residue was partitioned between water and EtOAc. The EtOAc layer was washed with saturated NaHCO3, water, brine, dried over anhydrous Na2SO4, filtered and concentrated to yield a brown oil. The crude material (the oil) was then purified by column chromatography (silica gel, hexanes:EtOAc 1:1 as eluent) to yield the title compound as a white solid.

1. customwas sealed in a tube
2. temperatureThe reaction mixture was cooled
3. customthe residue was partitioned between water and EtOAc
4. washThe EtOAc layer was washed with saturated NaHCO3, water, brine
5. dry with materialdried over anhydrous Na2SO4
6. filtrationfiltered
7. concentrationconcentrated
8. customto yield a brown oil
9. customThe crude material (the oil) was then purified by column chromatography (silica gel, hexanes:EtOAc 1:1 as eluent)