2-氰乙基（E）-3-氨基丁-2-烯酸酯

反应条件: temp:0.00; pressure:0.00; stir:

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

实验步骤: 280 g (0.63 mol) of cyclopentyl 2-acetyl-3-(2-chloro-6-fluorophenyl)-2-propenoate are dissolved with 97.2 g (0.63 mol) of 2-cyanoethyl 3-amino-2-butenoate in 400 ml of isopropanol and the solution is heated under reflux for about 8 hours until monitoring by thin layer chromatography (silica gel, toluene/ethyl acetate 5:1) shows complete conversion. The reaction mixture is concentrated and the residue is taken up twice more with toluene and the mixture concentrated again. Filtration twice over 2 l of silica gel each time using a toluene/ethyl acetate gradient gives 160 g of the target compound as an oil. A portion is further purified by chromatography over silica gel and crystallization from ether to give a crystalline solid of melting point 135-136° C. the solution is heated The reaction mixture is concentrated the mixture concentrated again Filtration twice over 2 l of silica gel each time

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

实验步骤: 280 g (0.63 mol) of cyclopentyl 2-acetyl-3-(2-chloro-6-fluorophenyl)-2-propenoate are dissolved with 97.2 g (0.63 mol) of 2-cyanoethyl 3-amino-2-butenoate in 400 ml of isopropanol and the solution is heated under reflux for about 8 hours until monitoring by thin layer chromatography (silica gel, toluene/ethyl acetate 5:1) shows complete conversion. The reaction mixture is concentrated and the residue is taken up twice more with toluene and the mixture concentrated again. Filtration twice over 2 l of silica gel each time using a toluene/ethyl acetate gradient gives 160 g of the target compound as an oil. A portion is further purified by chromatography over silica gel and crystallization from ether to give a crystalline solid of melting point 135-136° C. the solution is heated The reaction mixture is concentrated the mixture concentrated again Filtration twice over 2 l of silica gel each time

反应条件: temp:0.00; pressure:0.00; stir:

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

实验步骤: To 10 mL of methanol was added 20 g (0.13 mole) of 2-cyanoethyl acetoacetate. The solution was cooled in ice and a slow stream of ammonia gas was passed through it for five hours. The reaction flask was stoppered and stored at 0° C. overnight. The resulting solid was collected, washed with a small amount of methanol and dried under high vacuum to give 11.1 g (0.072 mole) of 2-cyanoethyl 3-aminobut-2-enoate, 1H NMR 4.6 (s, 1H), 4.3 (t, 2H), 2.8 (t, 2H), 2.0(t, 3H). The solution was cooled in ice The resulting solid was collected washed with a small amount of methanol dried under high vacuum

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

实验步骤: 280 g (0.63 mol) of cyclopentyl 2-acetyl-3-(2-chloro-6-fluorophenyl)-2-propenoate are dissolved with 97.2 g (0.63 mol) of 2-cyanoethyl 3-amino-2-butenoate in 400 ml of isopropanol and the solution is heated under reflux for about 8 hours until monitoring by thin layer chromatography (silica gel, toluene/ethyl acetate 5:1) shows complete conversion. The reaction mixture is concentrated and the residue is taken up twice more with toluene and the mixture concentrated again. Filtration twice over 2 l of silica gel each time using a toluene/ethyl acetate gradient gives 160 g of the target compound as an oil. A portion is further purified by chromatography over silica gel and crystallization from ether to give a crystalline solid of melting point 135-136° C. the solution is heated The reaction mixture is concentrated the mixture concentrated again Filtration twice over 2 l of silica gel each time