Ethyl Acetoacetate → HCID 178472877, Verbindung

Beteiligte Stoffe

Reaktionsschritte

To a solution of ethyl acetoacetate (compound 7, 30 g, 0.23 mol) in acetic acid (35 mL) was added slowly sodium nitrite (18.0 g, 0.25 mol) in cold water (40 mL) at −10° C. The reaction mixture was stirred for 1 hr, then added cold water (120 mL) and stirred for 3 hrs. The mixture was extracted with diethyl ether (300 mL). The organic layer was washed with saturated NaHCO3 (400 mL×2), then dried over anhydrous MgSO4, filtered and concentrated in vacuo. The obtained product (21.46 g, white solid) was used for the next step without purification.

Herkunft & Nachweise