反应详情

温度

50 °C

To a solution of ethylacetoacetate (2.7 kg, 20.74 mol) in ethanol (4 L) was added conc.H2SO4 (4 ml) at 25° C. under a nitrogen atmosphere. The mixture was heated to 50° C. before adding triethylorthoformate (3073.6 g, 20.74 mol) drop wise. The mixture was stirred at 50° C. for 16 h. The mixture was concentrated under reduced pressure to give the title compound (2.8 kg, 85%) as a yellow oil. 1H NMR (400 MHz, CDCl3): δ 4.9 (s, 1H), 4.1 (m, 2H), 3.7 (m, 2H), 2.2 (s, 3H), 1.2 (m, 3H), 1.1 (m, 3H).

1. customat 25° C.
2. concentrationThe mixture was concentrated under reduced pressure