反应详情

温度

0 °C

The 2-(1-propyn-1-yl)piperazine bis(trifluoroacetate (110 mg, 0.312 mmol) was dissolved in CH2Cl2 in a 50 mL round-bottomed flask and was then cooled to 0° C. To this solution was added an excess of triethylamine (152 μL, 1.093 mmol) followed by thiophene-2-sulfonyl chloride (57.0 mg, 0.312 mmol, Sigma-Aldrich, St. Louis, Mo.). The mixture was warmed slowly to room temperature and stirred for 2 h. Afterwards, the mixture was concentrated and absorbed onto silica gel. The crude material was purified via column chromatography (about 40 g silica gel, 0% to 10% MeOH in CH2Cl2) to give 3-(1-propyn-1-yl)-1-(2-thiophenylsulfonyl)piperazine (42 mg) as a foamy solid.

1. temperatureThe mixture was warmed slowly to room temperature
2. concentrationAfterwards, the mixture was concentrated
3. customabsorbed onto silica gel
4. customThe crude material was purified via column chromatography (about 40 g silica gel, 0% to 10% MeOH in CH2Cl2)