Chloroacetone → HCID 10954610, compound

Participants

Reaction Steps

165.8 g (1.2 mol) of potassium carbonate and 4.6 g (0.02 mol) of benzyltriethylammonium chloride are suspended in 500 ml of acetonitrile. While stirring there are added thereto 146.1 g (1 mol) of methyl 4-methoxy-acetoacetate and there are added dropwise thereto within 10 minutes 138.8 g (1.5 mol) of chloroacetone. The mixture is stirred at 20°-25° C. for a further 7 hours. The reaction mixture is poured on to 1 liter of 10% NaH2PO4 solution/ice (pH value=5) and extracted 3 times with 500 ml of ethyl acetate each time. The combined organic phases are dried over magnesium sulphate and concentrated on a rotary evaporator to give 206.30 g (100%) of methyl 4-methoxy-2-acetonylacetoacetate, content: 84.3%; b.p. 104°-105° C./0.06 mbar.

Provenance & Evidence