反应详情

温度

60 °C

220 mg (0.38 mmol) 5-Chloro-thiophene-2-carboxylic acid (2-{(1-isopropyl-piperidin-4-yl)-[3-(tetrahydro-pyran-2-yloxy)-propyl]-sulfamoyl}-ethyl)-amide were dissolved in a mixture of 4 ml THF, 8 ml conc. acetic acid and 2 ml water. The resulting mixture was stirred for 8 h at 60° C., concentrated under reduced pressure and purified by preparative RP-HPLC (CH3CN/H2O gradient+0.1% TFA). The product was taken up in dichloromethane and treated with a saturated NaHCO3-solution. After phase separation the organic phase was concentrated and the resulting residue was dissolved in water containing 1 equiv. of fumaric acid. Lyophilisation gave the title compound as its fumarate in form of a colorless amorphous material.

1. concentrationconcentrated under reduced pressure
2. custompurified by preparative RP-HPLC (CH3CN/H2O gradient+0.1% TFA)
3. additiontreated with a saturated NaHCO3-solution
4. customAfter phase separation the organic phase
5. concentrationwas concentrated