in bulk supply 66981-73-5 for sale Tianeptine Sodium best quality

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in bulk supply 66981-73-5 for sale Tianeptine Sodium best quality

Preparation of the first step: to 5L reaction bottle, in order to add 540g (3,11-dichlorine-6, 11-dihydro-6-methyl-diphenyl-diphenyls-c, f) 1,2) sulfur-nitrogen hybrid-5,5 -dioxide), 433g7-ethyl ethyl acid hydrochloride, 2500ml acetylene, 370g triethylamine, heated to 50C-60C after 2 hours of insulation, decompression concentrate dry; Water 1L stirred for 0.5 hours, static layering, take organic layer, and then wash with water 1L, combined machine phase, decompression concentrated viscosity 7-(3-chlorine-6, 11-dihydro-5,2 5-Dioxy-6-Methyl diphenyl (c,f) (1,2) ethyl acid brown viscose 600g, yield 81%, purity 98%.

Step 2: The above-mentioned viscosity will be added to 1.4L ethanol stirring, add 450mL, 10% potassium hydroxide water solution, the reaction fluid PH ≥8, heating heating to 50-60 degrees C, reaction for 30 minutes, while constantly detecting the reaction fluid PH, if less than 8, need to add alkali liquid to ensure that the system pH value is greater than or equal to 8. After the reaction, decompression steamed out ethanol, added 600mL deionized water, 500mL dichloromethane, stirred, with concentrated hydrochloric acid, transferred to the material just layered, take organic phase, water phase with 500mL × 2 dichloromethane extraction, combined organic phase, decompression concentrated to dry. Add 5L waterless ethanol, heating dissolved, cooling to 5 degrees C stirring crystal 2 hours, filtration, filter cake 50 to 60 degrees C vacuum drying 20 to 24 hours, that is, the class of white powder niptin crude 500g. Its crude reheating solution is dissolved in 10 times the ethanol cooling crystal, filtration, dry nippentin sodium concentrate products 425g, yield 75%, purity 99.5%.