反应详情

温度

30 °C

The sulfonyl chloride compound obtained in Example II (338 gm, 1.3M) is suspended in dry dioxane (400 ml) under argon atmosphere in a four-necked round-bottomed flask equipped with a condenser, a thermowatch and a constant pressure addition funnel. Excess t-butylamine (210 gm, 2.78M) is added drop-wise and the temperature of the reaction mixture is allowed to increase to approximately 60°-70° C. When the addition of amine is complete, the reaction mixture is aged at 70° C. for one hour, then cooled to 30° C. and the amine hydrochloride salt is removed by filtration. Concentration of the filtrate yields the crude sulfonamide. Nmr spectra obtained on a Varian EM-360 MHz nmr spectrometer, recorded in ppm downfield from tetramethylsilane, and infrared spectra recorded on a Nicolet MX-1 Fourier Transform infrared spectrometer provides spectral data consistent with the expected structure.

1. customequipped with a condenser
2. additiona thermowatch and a constant pressure addition funnel
3. temperatureto increase to approximately 60°-70° C
4. customthe amine hydrochloride salt is removed by filtration