反应详情

温度

135 °C

A mixture of ethyl acetoacetate (100 g, 0.77 mol), triethyl orthoformate (130 g, 0.92 mol), and acetic anhydride (150 g, 1.5 mol) was heated at 135° C. for 6-18 h in a round bottomed flask that was equipped with a distillation apparatus to collect the ethanol generated during the reaction. The reaction was cooled, concentrated and the residue was distilled under high vacuum to obtain the desired product (100 g, 70%) as a pale yellow oil: ESI MS m/z 187 [M+H]+.

1. customwas equipped with a distillation apparatus
2. customto collect the ethanol
3. customgenerated during the reaction
4. temperatureThe reaction was cooled
5. concentrationconcentrated
6. distillationthe residue was distilled under high vacuum