4-溴-N-[2-(二甲氨基)乙基]苯甲酰胺

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:150.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A microwave vial containing 4-bromo-benzoic acid ethyl ester (1 g, 4.36 mmol) and N,N-dimethylethylenediamine (2.37 g, 21.38 mmol) was heated under microwave radiation (150° C., 10 min). The volatiles were removed under rotary evaporation and the crude was used in the next step without further purification. Yield: 1.18 g, 100%. LCMS method: 2, RT: 1.93 min; MI: 271-273 [M+1]. The volatiles were removed under rotary evaporation the crude was used in the next step without further purification

反应条件: temp:150.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A microwave vial containing 4-bromo-benzoic acid ethyl ester (1 g, 4.36 mmol) and N,N-dimethylethylenediamine (2.37 g, 21.38 mmol) was heated under microwave radiation (150° C., 10 min). The volatiles were removed under rotary evaporation and the crude was used in the next step without further purification. Yield: 1.18 g, 100%. LCMS method: 2, RT: 1.93 min; MI: 271-273 [M+1]. The volatiles were removed under rotary evaporation the crude was used in the next step without further purification

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:150.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A microwave vial containing 4-bromo-benzoic acid ethyl ester (Ig, 4.36 mmol) and N,N-dimethylethylenediamine (2.37 g, 21.38 mmol) was heated under microwave radiation (150° C., 10 min). The volatiles were removed under rotary evaporation and the crude was used in the next step without further purification. Yield: 1.18 g, 100%. LCMS method: 2, RT: 1.93 min; MI: 271-273 [M+1]. The volatiles were removed under rotary evaporation the crude was used in the next step without further purification

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

实验步骤: 4-Bromophenylcarboxylic acid (100.0 mg, 0.497 mmol), 100.8 mg (0.746 mmol) of 1-hydroxybenzotriazole, 143.0 mg (0.746 mmol) of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride, and N,N-dimethylformamide (1.0 ml) were added in that order, and the mixture was stirred at room temperature for 20 min. Thereafter, 0.080 ml (0.746 mmol) of N1,N1-dimethylethane-1,2-diamine was added thereto, and the mixture was stirred at room temperature for one hr. A saturated aqueous sodium hydrogencarbonate solution was added thereto, and the mixture was then extracted with ethyl acetate. The extract was dried over anhydrous sodium sulfate and was then filtered. The filtrate was concentrated under the reduced pressure, and the residue was purified by preparative thin-layer chromatography (chloroform:methanol:28% aqueous ammonia=9:2:0.2) to give 127 mg (yield 94%) of the title compound. the mixture was stirred at room temperature for one hr the mixture was then extracted with ethyl acetate The extract was dried over anhydrous sodium sulfate was then filtered The filtrate was concentrated under the reduced pressure the residue was purified by preparative thin-layer chromatography (chloroform:methanol:28% aqueous ammonia=9:2:0.2)

反应条件: temp:150.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A microwave vial containing 4-bromo-benzoic acid ethyl ester (1 g, 4.36 mmol) and N,N-dimethylethylenediamine (2.37 g, 21.38 mmol) was heated under microwave radiation (150° C., 10 min). The volatiles were removed under rotary evaporation and the crude was used in the next step without further purification. Yield: 1.18 g, 100%. LCMS method: 2, RT: 1.93 min; MI: 271-273 [M+1]. The volatiles were removed under rotary evaporation the crude was used in the next step without further purification