反应详情

A solution of 4-methoxy-6-trifluoromethylpyran-2-one (2.7 g, 14 mmol) in a methanolic magnesium methanolate solution (8.5% Mg(OMe)2, 8.36 g, 8 mmol) was heated under reflux for 16 hours. The solution was concentrated and taken up in water and ethyl acetate, and the organic phase was brought to pH 5 by adding dilute hydrochloric acid. The organic phase was separated off, dried and concentrated. 1.5 g of crude product were obtained as a yellow oil. Kugelrohr distillation at 0.04 mbar and about 160° C. afforded methyl 6,6,6-trifluoro-3-methoxy-5-oxo-2-hexenoate (1.50 g, 6.6 mmol, 48%) as a pale yellow oil.

1. temperatureunder reflux for 16 hours
2. concentrationThe solution was concentrated
3. additionby adding dilute hydrochloric acid
4. customThe organic phase was separated off
5. customdried
6. concentrationconcentrated
7. custom1.5 g of crude product were obtained as a yellow oil
8. distillationKugelrohr distillation at 0.04 mbar and about 160° C.