Hydrochloric Acid → HCID 67087966, compound

Participants

Reaction Steps

11.2 ml (98 mmol) of dimethyl malonate were slowly added dropwise to a suspension, cooled to 10° C., of 3.56 g (89 mmol) of sodium hydride (60% dispersion in mineral oil) in 150 ml of dimethylformamide, and the mixture was then stirred at room temperature for 30 minutes. Subsequently, 9.6 g (30 mmol) of 3,5-dichloro-3-(2-ethoxypyridin-3-yl)-1,3-dihydroindol-2-one from example 1.1 were added in portions, and the mixture was stirred at room temperature for 15 min. To work up the reaction it was stirred into cold 1N HCl, and dichloromethane was added. The phases were separated, and the aqueous phase was extracted with dichloromethane. The combined organic phase was washed with water and saturated sodium chloride solution and dried over magnesium sulfate, and the solvent was removed in vacuo. The residue was recrystallized from dichloromethane/pentane. 9.01 g of the title compound were obtained as a yellowish solid.

Provenance & Evidence