Green Synthesis Technique Of Medical Intermediate DM

This research takes the industrial M as the raw material, adopting the greenoxidant—hydrogen peroxide, using the nontoxic and low noxious organic reagent, theone-step method synthesized the high-quality DM. The product can immediately meetthe request in medicine production, the technology is feasible. Make use of the IRspectrum to analyze the outcome; make use of the melting point apparatus and HPLCto analyze the product's purity. At the same time, reclaim the organic reagent,simulate and validate the whole reclaim flow. Make sure that the reagent can beused circularly; the whole process is low cost and cleanly.By a great deal of experiment, the optimum technologic condition is:Take IPA as the organic reagent, oxidizing the M- Na solution to get DM, themelting point can arrive at 180℃, Yield 80～90ï¼…; The optimum technologic conditionis: reaction temperature 50℃, addition time 1 h, reaction time 1.5 h, the concentrationof M- Na solution 30ï¼…, the ratio of materials 2:1, the excess of alkali 5ï¼…, the quantityof reagent 1.5 times;( based on the quantity of M- Na solution);Take IPA as the organic reagent, oxidizing the solid M to get DM, the meltingpoint can arrive at 181℃, Yield 90ï¼…; The optimum technologic condition is: additiontime 1.25 h, the ratio of material 2:1.2, reaction temperature 50℃, the ratio betweenthe quantity of reagent and M 7, the ratio of reagent in hydrogen peroxide 1 : 3 ( basedon the quantity of M);Take THO as the organic reagent, oxidizing the solid M to get DM, the meltingpoint can arrive at 184.5℃, Yield 96ï¼…, purity 99.6ï¼…; The optimum technologiccondition is: reaction temperature 40℃, addition time 1 h, reaction time 3h, thequantity of Na₂CO₃ 2.5ï¼…(based on M), the ratio of material is 2:1.1, the quantity of reagent 3times (based on the quantity of M), deposited time Oh;At the same time, the addition of molecule sieve and surfactant can raise thefield, but make no difference to the melting point.Use the ASPAN software to simulate and calculate the organic reagent reclaimflow, the optimum technologic parameter of the extract distillation is: the number ofboard of extract distillation column 22, the feed plate 19, the location of solventfeed-in 3, the temperature of solvent 40℃, the temperature of raw material 50℃,reflux ratio 0.8, molecular rate of solvent and raw material 0.65; The number of boardof solvent reclaim column 13, the feed plate 6, reflux ratio 0.5. By batch extractdistillation experiment, the content of outcome is analyzed by GC; the purity isaccordant to the simulation.