反应详情

温度

105 °C

A suspension of N-(4-chlorobenzyl-4-hydroxy-6-(4-morpholinylmethyl)-3-quinolinecarboxamide (0.25 gm) from Preparation No. 40 and cesium carbonate (0.39 gm) in DMF (3 mL) is treated with chloromethyl 4-chlorophenyl sulfide (0.13 mL). The mixture is tightly capped and heated to 105° C. for 2 hrs. The reaction mixture is allowed to cool to room temperature, diluted with dichloromethane (50 mL), washed with water (2×10 mL), brine, dried (Na2SO4) and concentrated under reduced pressure. The crude product is purified by flash column chromatography eluting with 1% to 3% methanol in dichloromethane and then by trituration with ethyl acetate to afford 0.26 gm of the title compound as a white solid.

1. customfrom Preparation No
2. customThe mixture is tightly capped
3. temperatureto cool to room temperature
4. washwashed with water (2×10 mL), brine
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated under reduced pressure
7. customThe crude product is purified by flash column chromatography
8. washeluting with 1% to 3% methanol in dichloromethane