反应详情

温度

110 °C

A mixture of 100 mg 5-{6-[3-(4-fluorophenyl)-1-trityl-1H-pyrazol-4-yl]quinazolin-4-yl}thiophen-2-sulfonic acid (2-chloroethyl)methylamide (compound in Example 746), 29 μL 1-methyl piperazine, 72 μl triethylamine and 3 mL N,N-dimethylformamide was stirred at 110° C. for 24 hours. Ethyl acetate and water were added to the reaction solution, and the organic layer was separated. The organic layer was washed with water and brine and dried over sodium sulfate, and the solvent was evaporated. The residue was purified by NH silica gel column chromatography (hexane/ethylacetate)to give 41 mg 5-{6-[3-(4-fluorophenyl)-1-trityl-1H-pyrazol-4-yl]quinazolin-4-yl}thio phen-2-sulfonic acid methyl-[2-(4-methylpiperazin-1-yl)ethyl]amide. This product was reacted in the same manner as in Example 68, to give 28 mg of the title compound as yellow crystals.

1. customthe organic layer was separated
2. washThe organic layer was washed with water and brine
3. dry with materialdried over sodium sulfate
4. customthe solvent was evaporated
5. customThe residue was purified by NH silica gel column chromatography (hexane/ethylacetate)