反应详情

To a solution of 80 mg of 1-(1-ethyl-propyl)-2-thiophen-2-ylmethyl-1H-benzoimidazole-5-carboxylic acid in 0.5 ml of dry DMF 17 mg of HOAT, 56 mg of EDC and 0.24 ml of DIPEA were added at 0° C. After 15 min 60 mg of (S)-2-Amino-4-methyl-pentane-1-sulfonic acid methylamide-hydrochloride were added and the reaction was stirred at it for 20 h. The reaction was then poured into water and the pH was adjusted to 3 by the addition of 2 M aqueous hydrochloric acid. The reaction was extracted with ethyl acetate three times. The combined organic phases were washed with 2 M aqueous hydrochloric acid, saturated sodium bicarbonate solution and brine, dried over magnesium sulphate and concentrated. After purification by HPLC 55 mg (45%) of 1-(1-Ethyl-propyl)-2-thiophen-2-ylmethyl-1H-benzoimidazole-5-carboxylic acid ((S)-3-methyl-1-methylsulfamoylmethyl-butyl)-amide were obtained.

1. extractionThe reaction was extracted with ethyl acetate three times
2. washThe combined organic phases were washed with 2 M aqueous hydrochloric acid, saturated sodium bicarbonate solution and brine
3. dry with materialdried over magnesium sulphate
4. concentrationconcentrated
5. customAfter purification by HPLC 55 mg (45%) of 1-(1-Ethyl-propyl)-2-thiophen-2-ylmethyl-1H-benzoimidazole-5-carboxylic acid ((S)-3-methyl-1-methylsulfamoylmethyl-butyl)-amide
6. customwere obtained