反应详情

温度

0 °C

To a stirred solution of ethyl acetoacetate (25 g) in tetrahydrofuran (800 ml) at 0° C. was added LDA (2.0M solution in heptanes/tetrahydrofuran/ethylbenzene) (194 ml). After 40 min the product from step (ii) (39 g) was added dropwise and the mixture was stirred at 0° C. for 1 hour. The reaction mixture was acidified with 2N HCl and the organic phase was concentrated under reduced pressure. The residue was dissolved in diethyl ether and washed with water and saturated brine. The organic phase was collected, dried (MgSO4) and evaporated under reduced pressure. Purification was by chromatography eluting with 5-10% ethyl acetate in isohexane.

1. concentrationthe organic phase was concentrated under reduced pressure
2. dissolutionThe residue was dissolved in diethyl ether
3. washwashed with water and saturated brine
4. customThe organic phase was collected
5. dry with materialdried (MgSO4)
6. customevaporated under reduced pressure
7. customPurification
8. washeluting with 5-10% ethyl acetate in isohexane