Hydrochloric Acid → HCID 178431788, compound

Participants

Reaction Steps

To a slurry of ethyl 2-methyl-3-oxobutanoate (10 g, 69.4 mmol, 1 equiv) and 2-cyanoacetamide (5.8 g, 69.4 mmol, 1 equiv) was slowly added a solution of KOH (4.9 g, 87 mmol, 1.25 equiv) in MeOH (35 mL). Stir for 1 h during which time solution became homogenous yellow before developing a cream colored precipitate. Heat at reflux for 3 h. Upon cooling to ambient temperature, concentrated HCl (9 mL) was added. The off white solid was filtered and washed with ether to provide the product (10.7 g, 94%) as a cream colored solid. 1H NMR (500 MHz, DMSO-d6) δ 2.22 (s, 3H), 1.90 (s, 3H); LCMS (ESI, M+1): 165.05.

Provenance & Evidence