Potassium Carbonate → HCID 66523188, compound

Participants

Reaction Steps

Ethyl 4-Cyclopropyl-3-[(methoxyacetyl)amino]-4-oxobutanoate (Preparation 121, 25.7 g, 0.1 mol) was dissolved in dry DMF (170 mL). POCl3 (46 g, 0.3 mol) was poured into this solution at 5-15° C., and the mixture was kept this temperature for 60 minutes. The resulting solution was slowly poured in portions into crushed ice (700 g) and stirred until a homogeneous solution was obtained. The solution was neutralized with a 20% aqueous K2CO3 solution to pH 7-8. The product was extracted with ethyl acetate. The organic extract was washed with brine and concentrated in vacuo to give a dark-brown liquid, which was purified by silica gel column chromatography eluting with EtOAc:Hexane 1:1 to afford the title compound as a colourless liquid (96%). Taken directly on to the next step.

Provenance & Evidence