多巴胺EP杂质B

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

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: 1.7 g of 2-(4-hydroxy-3-methoxy-phenyl)-ethylamine and 2.1 g of (S)-2-(ethylsulfonylamino)-3-methyl-butyric acid are stirred at room temperature for 2 hours together with 4.6 g of (benzotriazol-1-yl)-tris(dimethylamino)phosphonium hexafluorophosphate and 4.5 ml of diisopropylethylamine in 40 ml of dimethylformamide. The reaction mixture is then introduced into 600 ml of water. Extraction is carried out twice using 400 ml of ethyl acetate each time. The organic phases are washed twice using 300 ml of water each time and once with 200 ml of saturated sodium chloride solution, dried over magnesium sulfate and concentrated, yielding (S)-2-(ethylsulfonylamino)3-methyl-butyric acid N-[2-(4-hydroxy-3-methoxyphenyl)-ethyl]-amide in the form of a brown oil, which can be purified by chromatography on silica gel with ethyl acetate. Extraction The organic phases are washed twice once with 200 ml of saturated sodium chloride solution, dried over magnesium sulfate concentrated

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

实验步骤: A mixture of 2.1 g of (S)-2-(ethylsulfonylamino)-3-methyl-butyric acid, 1.7 g of 2-(4-hydroxy-3-methoxyphenyl)-ethylamine, 4.6 g of (benzotriazol-1-yloxy)-tris(dimethylamino)phosphonium hexafluorophosphate (BOP) and 4.5 ml of N,N-diisopropylethylamine is stirred in 40 ml of N,N-dimethylformamide at room temperature for 2 hours. The reaction mixture is introduced into 500 ml of water and extracted twice with 400 ml of ethyl acetate each time. The organic phases are washed once with 300 ml of water and once with 200 ml of saturated sodium chloride solution, dried over magnesium sulfate and concentrated. (S)-2-(Ethylsulfonylamino)-3-methyl-butyric acid N-[2-(4-hydroxy-3-methoxyphenyl)-ethyl]-amide is obtained in the form of an oil, which can be purified by flash-chromatography on silica gel using a mixture of ethyl acetate/n-hexane=3:1. extracted twice with 400 ml of ethyl acetate each time The organic phases are washed once with 300 ml of water and once with 200 ml of saturated sodium chloride solution dried over magnesium sulfate concentrated