(E)-3-环己基-2-丙酸乙酯

反应条件: temp:-78.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Add triethylphospinoacetate (185 g, 821 mmol) to a suspension of hexane-washed sodium hydride (34.5 g, 60%, 862 mmol) in THF (1 L) at 0° C. Stir the resulting mixture for 1 h, and then cool it to −78° C. Then add a solution of cyclohexylmethanal (92.2 g, 821 mmol) in THF (500 mL) dropwise over 90 min, maintaining an internal temperature of less than −68° C. Allow the reaction mixture to warm to r.t. over 18 h. Then add a solution of saturated aqueous ammonium chloride solution (1 L) to the reaction mixture carefully. Extract the resulting mixture with ether (3×1 L). Combine the extracts and wash them with water (2×1 L), followed by saturated aqueous sodium chloride solution (1 L). Then dry the extracts over magnesium sulfate, and concentrate the solution under vacuum to afford the title compound as a yellow oil (154.8 g). GC-MS (m/e): 182 (M+). maintaining an internal temperature of less than −68° C to warm to r.t. over 18 h Extract the resulting mixture with ether (3×1 L) Combine the extracts and wash them with water (2×1 L) Then dry the extracts over magnesium sulfate concentrate the solution under vacuum