Synthesis and post-processing method of sulpiride or optical isomer thereof
A technology of optical isomers and inert gases, applied in the field of medicine, can solve problems such as unfavorable large-scale production, time-consuming and labor-intensive, difficult filtration and washing, and achieve the effect of meeting quality requirements, avoiding impurities, and easy post-processing
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Embodiment 1
[0025] Add 49g of 2-methoxy-5-sulfamoylbenzoic acid methyl ester and (S)-1-ethyl-2-aminomethyltetrahydropyrrolidine 26.5g into the reaction flask, under the protection of nitrogen at 90-100 ℃ for 5 hours, the reaction was completed, cooled to 80 ℃, added 50g of ethanol, stirred and refluxed for 10 minutes, cooled to 5 ℃ and stirred for 2 hours, filtered, washed with ethanol, and dried at 65 ℃. Yield 93.8%, purity 99.2%.
Embodiment 2
[0027] Add 25.9 g of ethyl 2-methoxy-5-sulfamoylbenzoate, 15 g of (S)-1-ethyl-2-aminomethyltetrahydropyrrolidine and 20 g of isopropanol into the reaction flask, 80 ℃ for 36 hours, the reaction is over, add 10 g of ethanol, stir and reflux for 10 minutes, cool to 5 ℃ and stir for 1 hour, filter, wash with ethanol, and dry at 65 ℃. Yield 90.3%, purity 99.1%.
Embodiment 3
[0029] Add 123g of 2-methoxy-5-sulfamoylbenzoic acid methyl ester, 75g of 1-ethyl-2-aminomethyltetrahydropyrrolidine and 100g of ethylene glycol into the reaction flask. React at 100°C for 4-6 hours. When the reaction is over, cool naturally to 80°C, add 190g of ethanol, stir and reflux for 5 minutes, cool to 0°C and stir for 2 hours, filter, wash with ethanol, and dry at 65°C. Yield 85.1%, purity 99.5%.
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