Method for preparing isosulfan blue
A technology of isosulfide blue and acid blue, applied in the field of preparation of isosulfide blue, can solve the problems of difficult metal content, high price of silver oxide, large environmental pollution, etc., and achieves convenient large-scale production, low cost, and safety. high effect
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[0023] The invention provides a preparation method of isosulfur blue, comprising the following steps, S1, under the condition of 5-10°C, adding sodium chlorite and acid blue with a molar ratio of 2.5:1.0-3.5:1.0 into the reaction bottle , and an acid solution with an equivalent concentration of 5.0N to 12.0N for reaction, and the reaction time is 6 to 10 hours. The mass ratio of the volume of the acidic solution to the acid blue is 5.0:1.0-8.0:1.0. The acidic solution is sulfuric acid, phosphoric acid, methanesulfonic acid, p-toluenesulfonic acid, trifluoroacetic acid. The normality of the acidic solution is preferably 6.0N-8.0N.
[0024] S2, obtain isothiocyanine free acid crude product after completion of the reaction;
[0025] S3, dissolving the prepared crude isothiocyanate free acid in deionized water, and adjusting the pH to 8-9 through saturated aqueous sodium bicarbonate solution;
[0026] S4. Recrystallize the pH-adjusted solution in S3, filter, wash, and dry to ob...
example 1
[0030] Add acid blue (10.0g, 18.0mmol), sodium chlorite (4.9g, 54.0mmol), water (75ml), phosphoric acid (75ml), react at 5~10°C in the dark for 10 hours, after the reaction is completed, filter to obtain 10g of crude isothiocyanic acid; dissolve the crude product in deionized water (30ml), adjust the pH to 8-9 with saturated sodium bicarbonate solution, add acetone (300ml), stir for 1h;
[0031] Filter, wash the filter cake twice with acetone (150ml), and dry it in vacuum at 40°C for 8h to obtain 5.5g of isosulfur blue,
[0032] The purity is 99.6%, the unknown single impurity is <0.10%, and the yield is 53%.
[0033] The infrared spectrum of the sample is completely consistent with the standard spectrum.
[0034] 1 HNMR (solvent DMSO; internal standard TMS): δ1.19-1.23(t, 12H), δ3.60-3.65(q, 8H), δ6.97-6.99(d, 4H), δ7.13(s, 1H) ), δ7.28-7.30(d, 4H), δ7.72-7.74(d, 1H), δ7.88-7.90(d, 1H) .
example 2
[0036] Add acid blue (10.0g, 18.0mmol), sodium chlorite (4.9g, 54.0mmol), water (75ml), and Sulfuric acid (75ml), react in the dark at 5~10°C for 8 hours, filter the crude product of isothiocyanic acid 10g after the reaction is completed; dissolve the crude product in deionized water (30ml), adjust the pH to 8-9 with saturated sodium bicarbonate solution, add Acetone (300ml), stirred for 1h; filtered, the filter cake was washed twice with acetone (150ml), and vacuum-dried at 40°C for 8h to obtain 6.5g of isothiocyanine, with a purity of 99.7%, an unknown simplex <0.10%, and a yield of 63%.
[0037] The infrared spectrum of the sample is completely consistent with the standard spectrum.
[0038] 1 HNMR (solvent DMSO; internal standard TMS): δ1.19-1.23(t, 12H), δ3.60-3.65(q, 8H), δ6.97-6.99(d, 4H), δ7.13(s, 1H) ), δ7.28-7.30(d, 4H), δ7.72-7.74(d, 1H), δ7.88-7.90(d, 1H) .
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