Method for preparing S-(alpha, alpha-dimethyl benzyl) piperidine-1-thiocarboxylic
A technology of thioformate and dimethylbenzyl, applied in the field of preparation of S-piperidine-1-thioformate, can solve problems such as unfavorable industrialized production, achieve improved production environment and high yield , the effect of reducing production costs
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Embodiment 1
[0028] Into a 1000 ml four-neck round bottom flask equipped with a cooler, a thermometer, and an electric stirrer, add 600 ml (5.2 moles) of toluene and 103 g (1.21 moles) of piperidine, start stirring, and add dropwise at a temperature of 50 to 80°C Concentrated hydrochloric acid 147 g (solute content 1.21 moles), after the addition, the temperature was raised and refluxed to separate the water phase to obtain a toluidine hydrochloride solution; set aside. Put the above-mentioned piperidine hydrochloride solution into a 1000 ml four-neck flask again, pass gas phosgene at 60-90°C, and react for 6 hours. After the reaction liquid becomes clear, pass N 2 Drive off excess phosgene. The mother liquor was distilled to remove toluene to obtain 170 g of transparent pipecoyl chloride intermediate, the content of which was detected by gas chromatography was 98.3%, and the reaction yield was 95.5%.
[0029] In a 1000 ml four-necked flask, put 520 ml (4.5 moles) of toluene and 80 grams ...
Embodiment 2
[0031] Into a 1000 ml four-necked round bottom flask equipped with a cooler, a thermometer, and an electric stirrer, add 600 ml (5.2 moles) of toluene and 103 g (1.21 moles) of piperidine, start stirring, and add dropwise at a temperature of 20 to 90°C Concentrated hydrochloric acid 160 g (1.31 mol), after the addition, the temperature was raised and refluxed to separate the water phase to obtain a toluidine hydrochloride solution; set aside. Put the above-mentioned piperidine hydrochloride solution into a 1000 ml four-necked flask, and pass gas phosgene at 20-100°C. After reacting for 6 hours, the reaction solution becomes clear, and then pass N 2 Drive off excess phosgene. Toluene was removed from the mother liquor by distillation to obtain 170 g of transparent pipecoyl chloride intermediate, the content of which was detected by gas chromatography was 98.8%, and the reaction yield was 95.8%.
[0032] In a 1000 ml four-necked flask, add 520 ml (4.5 moles) of toluene and 8.0 ...
example 3
[0034]Into a 1000 ml four-neck round bottom flask equipped with a cooler, a thermometer, and an electric stirrer, add 600 ml (5.2 moles) of toluene and 103 g (1.21 moles) of piperidine, start stirring, and add dropwise at a temperature of 50 to 80°C Concentrated hydrochloric acid 147 g (solute content 1.21 moles), after the addition, the temperature was raised and refluxed to separate the water phase to obtain a toluidine hydrochloride solution; set aside. Put the above-mentioned piperidine hydrochloride solution into a 1000 ml four-neck flask again, pass gas phosgene at 60-90°C, and react for 6 hours. After the reaction liquid becomes clear, pass N 2 Drive off excess phosgene. The mother liquor was distilled to remove toluene to obtain 170 g of transparent pipecoyl chloride intermediate, the content of which was detected by gas chromatography was 98.2%, and the reaction yield was 95.4%.
[0035] In a 1000 milliliter four-necked flask, 520 milliliters (4.5 moles) of toluene a...
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