对氯苯丙酸乙酯

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

实验步骤: To dry toluene (4 ml) under an inert atmosphere at 0° C. was added a toluene solution of trimethylaluminium (2.45 ml, 4.89 mmol, 2 M solution). A solution of ethylenediamine (0.30 ml, 4.89 mmol) in toluene (1.5 ml) was then added dropwise and the reaction mixture was then allowed to warm to room temperature and stirred for 1 h at this temperature before being re-cooled to 0° C. To this mixture was added dropwise a solution of 3-(4-chloro-phenyl)-propionic acid ethyl ester (0.52 g, 2.45 mmol) in toluene (3 ml). The reaction mixture was then heated at 95° C. for 45 min and then cooled first to room temperature and finally to 0° C. The mixture was quenched by dropwise addition of methanol (1 ml) and when all gas evolution had ceased the mixture was diluted with water and extracted twice with ethyl acetate. The combined organic extracts were dried over sodium sulphate, filtered and concentrated in vacuo. The residue was triturated in ether to yield a white solid (0.26 g, 50%) which was collected by filtration; MS (ISP): 211.0, 209.2 ([M+H]+.). before being re-cooled to 0° C The reaction mixture was then heated at 95° C. for 45 min cooled first to room temperature and finally to 0° C The mixture was quenched by dropwise addition of methanol (1 ml) and when all gas evolution was diluted with water extracted twice with ethyl acetate The combined organic extracts were dried over sodium sulphate filtered concentrated in vacuo The residue was triturated in ether

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

实验步骤: To a solution of (E)-3-(4-chloro-phenyl)-acrylic acid ethyl ester (0.37 g, 1.73 mmol) in ethyl acetate (10 ml) were added palladium on activated charcoal (18 mg) and zinc bromide (80 mg, 0.35 mmol). The reaction vessel was then pressurized with hydrogen gas to a pressure of 1 atmosphere and the mixture was stirred for 18 h. The catalyst was then removed by filtration, washing with ethyl acetate, and the filtrate was concentrated in vacuo to yield a colourless oil which was used for the next step without further purification; MS (ISP): 214.2, 212.1 ([M+H]+.). The catalyst was then removed by filtration washing with ethyl acetate the filtrate was concentrated in vacuo to yield a colourless oil which was used for the next step without further purification