反应详情

63.6 g (0.6 mol) of sodium carbonate and 2.3 g (0.01 mol) of benzyltriethylammonium chloride are suspended in 250 ml of acetonitrile. While stirring there are added thereto 87.0 g (0.5 mol) of methyl 4-acetoxyacetoacetate and there are added dropwise thereto within 5 minutes 69.4 g (0.75 mol) of chloroacetone. The mixture is stirred at 20°-25° C. for a further 46 hours. The reaction mixture is poured on to 1 liter of 10% NaH2PO4 solution/ice (pH value=5) and extracted 3 times with 300 ml of ethyl acetate each time. The combined organic phases are dried over magnesium sulphate and concentrated completely on a rotary evaporator to give 105.9 g (92%) of methyl 4-acetoxy-2-acetonylacetoacetate, content 76.9%; b.p. 119°-121° C./0.06 mbar.

1. additionare added
2. stirringThe mixture is stirred at 20°-25° C. for a further 46 hours
3. extractionextracted 3 times with 300 ml of ethyl acetate each time
4. dry with materialThe combined organic phases are dried over magnesium sulphate
5. concentrationconcentrated completely on a rotary evaporator