反应详情

1.66 g (12 mmol) of potassium carbonate and 0.04 g (0.2 mmol) of benzyltriethylammonium chloride are suspended in 5 ml of acetonitrile. While stirring there are added thereto 1.60 g (10 mmol) of methyl 4-methoxy-2-methylacetoacetate and there are then added dropwise thereto within 15 minutes 1.39 g (15 mmol) of chloroacetone. The mixture is stirred at 20°-25° C. for a further 21 hours. The reaction mixture is poured into 20 ml of 2N HCl (pH value=1) and extracted 3 times with 20 ml of ethyl acetate each time. The combined organic phases are dried over sodium sulphate and evaporated on a rotary evaporator. The crude product distils at 95° C./0.03 mbar. There results 0.83 g (38.4%) of methyl 4-methoxy-2-acetonyl-2-methylacetoacetate.

1. additionare added
2. stirringThe mixture is stirred at 20°-25° C. for a further 21 hours
3. extractionextracted 3 times with 20 ml of ethyl acetate each time
4. dry with materialThe combined organic phases are dried over sodium sulphate
5. customevaporated on a rotary evaporator
6. customThe crude product distils at 95° C./0.03 mbar