2-氰基己酸乙酸

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

实验步骤: 323 g of butyraldehyde and 422 g of ethyl cyanoacetate are dissolved in 750 ml of glacial acetic acid, 15 g of piperidine are added, and the reaction mixture is stirred, during which it warms to about 55° C. After the reaction mixture has been cooled to room temperature, 20 g of 5% Pd-C catalyst are added, and the mixture is then hydrogenated at 30° and an H2 pressure of 2 bar until the calculated amount of hydrogen has been taken up (about 7 hours). After the catalyst has been separated off, the hydrogenation solution is evaporated on a rotary evaporator, the residue is taken up in..methyl tertiary-butyl ether (MTB ether), and the solution is washed by shaking twice with water and subsequently with 5% NaHCO3 solution. The organic phase is dried and evaporated. The residue is distilled in vacuo (2×10-2 mbar) (62° C. to 78°), to give ethyl 2-butylcyanoacetate. warms to about 55° C is then hydrogenated at 30° (about 7 hours) After the catalyst has been separated off the hydrogenation solution is evaporated on a rotary evaporator methyl tertiary-butyl ether (MTB ether), and the solution is washed by shaking twice with water and subsequently with 5% NaHCO3 solution The organic phase is dried evaporated The residue is distilled in vacuo (2×10-2 mbar) (62° C. to 78°)

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

实验步骤: 323 g of butyraldehyde and 422 g of ethyl cyanoacetate are dissolved in 750 ml of glacial acetic acid, 15 g of piperidine are added, and the reaction mixture is stirred, during which it warms to about 55° C. After the reaction mixture has been cooled to room temperature, 20 g of 5% Pd-C catalyst are added, and the mixture is then hydrogenated at 30° and an H2 pressure of 2 bar until the calculated amount of hydrogen has been taken up (about 7 hours). After the catalyst has been separated off, the hydrogenation solution is evaporated on a rotary evaporator, the residue is taken up in..methyl tertiary-butyl ether (MTB ether), and the solution is washed by shaking twice with water and subsequently with 5% NaHCO3 solution. The organic phase is dried and evaporated. The residue is distilled in vacuo (2×10-2 mbar) (62° C. to 78°), to give ethyl 2-butylcyanoacetate. warms to about 55° C is then hydrogenated at 30° (about 7 hours) After the catalyst has been separated off the hydrogenation solution is evaporated on a rotary evaporator methyl tertiary-butyl ether (MTB ether), and the solution is washed by shaking twice with water and subsequently with 5% NaHCO3 solution The organic phase is dried evaporated The residue is distilled in vacuo (2×10-2 mbar) (62° C. to 78°)