1-piperidin-1-ylsulfonylpiperazine

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:70.01; pressure:0.00; stir:

実験手順: Dilution of the aliquot (2 uL) with DMSO (200 uL).

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The title compound was synthesized in analogy to example 1, from 5-(4-isopropyl-piperazine-1-carbonyl)-1H-indole-2-carboxylic acid hydrochloride (example 1, intermediate b), and 1-(piperidin-1-yl-sulfonyl)-piperazine to afford the desired product as a light-brown solid (87%). MS (ISP): 531.2 (M+H)+.

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of 0.5 g (1.20 mmol) 6-bromo-5-(1-isopropyl-piperidin-4-yloxy)-1H-indole-2-carboxylic acid hydrochloride in 8 mL N,N-dimethylformamide, 0.48 g (1.50 mmol) O-(benzotriazol-1-yl)-N,N,N′,N′-tetramethyluronium tetrafluoroborate, 0.31 g (1.33 mmol) 1-(piperidin-1-yl-sulfonyl)-piperazine and 1.0 mL (0.77 g, 6.0 mmol) N,N-diisopropylethylamine were added. After 2 h the solution was poured on 10% aqueous sodium bicarbonate solution, the phases were separated and the aqueous phase was extracted three times with ethyl acetate. The combined organic layers were washed three times with water followed by brine, dried over magnesium sulfate, filtered and evaporated. The residue was purified by flash chromatography twice on silica gel using a gradient of dichloromethane: methanol (100:0 to 50:50 v/v) as eluant, to afford 0.4 g (56%) of the title compound as a light-yellow foam. the phases were separated the aqueous phase was extracted three times with ethyl acetate The combined organic layers were washed three times with water dried over magnesium sulfate filtered evaporated The residue was purified by flash chromatography twice on silica gel using a gradient of dichloromethane: methanol (100:0 to 50:50 v/v) as eluant

反応条件: temp:0.00; pressure:0.00; stir: