FIELD: chemistry.
SUBSTANCE: invention relates to synthesis of biologically active compounds - insecticide: 2-dimethyl-amino-1,3-bis(phenylthiosulphonyl)propane (Bancol). First, 2-dimethylamino-1,3-dichloropane is obtained by reacting 33-38% aqueous dimethylamine (DMA) solution with allyl chloride (AC) in molar ratio DMA:AC of 1.1-1.5:1.0 for 3-4 hours at temperature of 50-55°C with formation of dimethyl allylamine hydrochloride and, without separation thereof, chlorinated at temperature of 7-13°C for 8-10 hours to obtain 1-dimethylamino-2,3-dichloropropane hydrochloride (1-DMA-2,3-DCP HC). After removing residual chlorine, the 1-DMA-2,3-DCP HC is neutralised with 44-46% aqueous alkali solution in molar ratio 1-DMA-2,3-DCP HC:alkali of 1:1.25-1.5 at room temperature to form 2-dimethylamino-1,3-dichloropropane (2-DMA-1,3-DCP). The 2-DMA-1,3-DCP is separated in form of an amine layer, dried, dissolved in isopropyl alcohol and condensed with sodium benzenethiosulphonate (BTSP) in molar ratio 2-DMA-1,3-DCP: BTSP of 1:2-2.04 for 1.5-2.5 hours at temperature of 70-79°C. The sodium chloride crystals formed are filtered off under a vacuum at 70-75°C. The reaction mass is cooled to 20-10°C and the end product is separated by filtering.
EFFECT: invention increases product output and simplifies the method for production thereof.
3 cl, 2 ex
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Authors
Dates
2013-04-27—Published
2011-06-24—Filed