Synthetic method of benzenesulfonate derivative
A technology of benzenesulfonate ester and synthesis method, which is applied in the field of synthesis of benzenesulfonate derivatives, can solve the problems of complex synthesis method, battery performance degradation, damage, etc., and achieve simple synthesis method and enhanced high and low temperature stability Effect
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[0019] Example 1
[0020] Add 1.0mol of phenol and 500ml of dichloromethane to the reaction flask respectively, add triethylamine with stirring, then lower the temperature to below 15℃, start adding 1.1mol of benzenesulfonyl chloride dropwise, after the drop, return to room temperature and continue to stir for 1h, then heat up Continue the reaction at reflux for 2h, and after the gas phase detection reaction is complete, it is treated with ice, separated into layers, dried and concentrated to obtain a crude product and then recrystallized to obtain a pure product 222.3g. The calculated product yield is 95%. The measured purity is 99.93%, the moisture content is 30ppm, the acid value is 34ppm, and the measured density is 1.277g / cm 3 , Boiling point is 375.4℃760mmHg, and its 1H NMR spectrum is as figure 1 As shown, the 13CNMR spectrum is as figure 2 Shown.
[0021] The synthetic route is:
[0022]
Example Embodiment
[0023] Example 2
[0024] Add 1.0 mol of allyl alcohol and 500 ml of dichloromethane to the reaction flask, add pyridine under stirring, then lower the temperature to below 15 ℃, start dropping 2.1 mol of benzene sulfonyl chloride, after dropping, return to room temperature and continue stirring for 1 hour, and then warm to The reaction was continued at reflux for 2 hours. After the gas phase detection reaction was complete, the reaction was thawed, separated into layers, dried and concentrated to obtain a crude product and then recrystallized to obtain a pure product of 189.3 g. The calculated product yield was 95.5%. The detection purity is 99.95%, the moisture content is 30ppm, the acid value is 40ppm, and its 1H NMR spectrum is as follows image 3 As shown, the 13C NMR spectrum is as Figure 4 Shown.
[0025] The synthetic route is:
[0026]
Example Embodiment
[0027] Example 3
[0028] Add 1.0 mol propargyl alcohol and 500 ml dichloromethane to the reaction flask, add triethylamine under stirring, and then lower the temperature to below 15 ℃, start dropping 2.1 mol of benzenesulfonyl chloride, after dropping, return to room temperature and continue stirring for 1 hour, then The temperature is raised to reflux and the reaction is continued for 2 hours. After the gas phase detection reaction is complete, it is treated with ice, separated into layers, dried and concentrated to obtain a crude product and then recrystallized to obtain a pure product of 187.77 g, with a calculated yield of 95.8%. The detected purity is 99.93%, the moisture content is 28ppm, the acid value is 36ppm, and the density is 1.244g / mL.
[0029] The synthetic route is:
[0030]
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