Hydrochloric Acid → HCID 67165601, compound

Participants

Reaction Steps

To a solution of 3-(S)-benzyl-8-(2-ethylbutyryl)-1,4,8-triazaspiro[4,5]decan-2-one (1.0 g, 2.9 mmol) in 40 mL of dry THF there was added sodium hydride (90 mg, 3.8 mmol) at room temperature and under a blanket of nitrogen. Following stirring over a period of 1 h at RT benzyl chloride (1.47 g, 11.6 mmol) was slowly added dropwise and the mixture was then heated over a period of 12 h under reflux. Following the addition of an aqueous saturated HCl solution (20 mL), the reaction mixture was isolated by filtration and the filtrate was extracted with EE (3×15 mL), and the combined organic phases were dried over Na2SO4. Following removal, by distillation, of the solvent, there was obtained the crude product as a yellow oil. Further purification was carried out by column chromatography. The product 1,3-(S)-dibenzyl-8-(2-ethylbutyryl)-1,4,8-triazaspiro[4,5]decan-2-one was obtained in a yield of 1.1 g (52%).

Provenance & Evidence