Process method for synthetizing tert-butyl sulfinamide
A technology of tert-butylsulfinamide and process method, which is applied in the field of synthesis of organic compounds, and achieves the effects of good process stability, reduced production cost, and easy procurement
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Embodiment 1
[0028] A kind of technical method of synthesizing tert-butyl sulfinamide, synthetic route is as follows:
[0029] The specific steps are:
[0030] Example 1
[0031] a) Synthesis of N-methyltriphenylamine: under argon protection, add triphenylchloromethane (0.1076 mol) to a 1-liter reaction flask equipped with mechanical stirring and cooling bath, and maintain the temperature at -50 Between -60°C, slowly feed 600mL of liquid ammonia, add toluene with 1% triphenylchloromethane mass as internal standard analysis, triphenylchloromethane internal standard analysis is less than 1%, and the reaction stops after 4-6 hours. The reaction solution was raised to room temperature, and the ammonia gas was volatilized. Add 500mL methyl tert-butyl ether (MTBE), wash the organic layer with 70g mass concentration of 10% sodium carbonate, wash the organic layer with 75g*2 water, dry and concentrate to obtain N-methyl Triphenylamine crude product 24g. 1.5*24g diethyl ether beating, filter a...
Embodiment 2
[0036] A kind of processing method of synthesizing tert-butylsulfinamide, reaction formula is as embodiment 1, and concrete steps are:
[0037] a) Synthesis of N-methyltriphenylamine: under the protection of argon, add triphenylchloromethane (0.1076 mol) to a 1-liter reaction flask equipped with mechanical stirring and cold bath, and maintain the temperature at -60 Between ~-70°C, slowly inject 600mL of liquid ammonia, add toluene with 1% mass of triphenylchloromethane as the internal standard analysis, the internal standard analysis of triphenylchloromethane is less than 1%, and the reaction stops after 4-6 hours. The reaction solution was raised to room temperature, and the ammonia gas was volatilized. Add 500mL ethyl acetate, wash the organic layer with 70g mass concentration of 10% sodium carbonate, wash the organic layer with 75g*2 water, dry and concentrate to obtain the crude product of N-methyltriphenylammonia 25.5 g. 1.5*25.5g n-hexane beating, filter after 1.5h, and...
Embodiment 3
[0042] A kind of processing method of synthesizing tert-butylsulfinamide, reaction formula is as embodiment 1, and concrete steps are:
[0043] a) Synthesis of N-methyltriphenylammonia: under the protection of argon, add triphenylbromethane (0.1076 mol) to a 1-liter reaction flask equipped with mechanical stirring and cold bath, and maintain the temperature at -60~ Between -70°C, slowly feed 600mL of liquid ammonia, add toluene with 1% mass of triphenylbromomethane as internal standard analysis, triphenylbromomethane internal standard analysis is less than 1%, and the reaction stops after 4-6 hours. The reaction solution was raised to room temperature, and the ammonia gas was evaporated. Add 500mL MTBE, wash the organic layer with 70g mass concentration of 10% sodium carbonate, wash the organic layer with 75g*2 water, dry and concentrate to obtain 26g of crude N-methyltriphenylamine. 1.5*26g of diethyl ether was beaten, filtered after 1.5h, and the dried product was 0.0930mol....
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