反应详情

To a suspension of 2 g of sodium hydride in 20 mL of THF, 2.4 g of 4-amino-3,5-dichloropyridine (15 mmoles) in 30 mL of THF are added dropwise at −5° C. The mixture is then kept for one hour at 20° C. with stirring. Subsequently, the previously prepared suspension of 1-(3-methoxybenzyl)-7-azaindole-3-yl-glyoxylic acid chloride is added dropwise at about 0° C. Finally, the reaction mixture is refluxed for 4 hours, after which the solvent is removed under vacuum. The residue is stirred with 50 mL of ethyl acetate and 50 mL of water. The phases are separated and the organic phase is washed with water. The solvent is distilled off under vacuum and the residue recrystallized from ispropanol.

1. additionare added dropwise at −5° C
2. additionis added dropwise at about 0° C
3. temperatureFinally, the reaction mixture is refluxed for 4 hours
4. customafter which the solvent is removed under vacuum
5. stirringThe residue is stirred with 50 mL of ethyl acetate and 50 mL of water
6. customThe phases are separated
7. washthe organic phase is washed with water
8. distillationThe solvent is distilled off under vacuum
9. customthe residue recrystallized from ispropanol