反应详情

温度

95 °C

A mixture of 8-methyl-2-piperazin-1-ylmethyl-2,3-dihydro-[1,4]dioxino[2,3-f]quinoline of Step B′ (0.493 g, 1.64 mmol) and 6-bromo-2-chloroquinoline of Example 1, Step A (0.507 g) is heated at 95° C. under nitrogen for 6 hours, followed by heating at 105° C. for 4 hours. The mixture is cooled, poured into saturated aqueous sodium bicarbonate and extracted with ethyl acetate. The extracts are dried over anhydrous magnesium sulfate and evaporated to dryness. The residue is flash chromatographed on silica Merck-60 using a gradient of methanol (0.5–2%) in dichloromethane-hexane (45:55), to provide the title compound (0.147 g) identical to the compound of Example 27, Step C.

1. temperatureby heating at 105° C. for 4 hours
2. temperatureThe mixture is cooled
3. extractionextracted with ethyl acetate
4. dry with materialThe extracts are dried over anhydrous magnesium sulfate
5. customevaporated to dryness
6. customchromatographed on silica Merck-60