反应详情

温度

-15 °C

To flame dried flask containing (E)-4-oxo-2-pentenoyl chloride (1.16 g, 8.76 mmol) in ether cooled to -15° C. is added diethylamine (1.41 g, 19.28 mmol) in ether (5 ml) and stirred for 2 hours while being warmed to ambient temperature. The solvents are removed in vacuo, and chromatographed on silica gel (230-400 mesh, 100 ml), eluting with hexane/ethyl acetate (75/25). The appropriate fractions are combined (Rf =0.31, TLC, hexane/ethyl acetate, 25/75) and concentrated in vacuo to give the title compound, NMR (CDCl3) 7.15, 7.04, 3.45, 3.40, 2.33, 1.20, 1.15.

1. temperatureTo flame
2. customdried flask
3. temperaturewhile being warmed to ambient temperature
4. customThe solvents are removed in vacuo
5. customchromatographed on silica gel (230-400 mesh, 100 ml)
6. washeluting with hexane/ethyl acetate (75/25)
7. concentrationconcentrated in vacuo