The preparation method and its usage of essentially pure methylene blue pentahydrate form A

The preparation method and its usage of essentially pure methylene blue pentahydrate form A

  • CN 102,666,510 B
  • Filed: 09/23/2010
  • Issued: 09/14/2016
  • Est. Priority Date: 09/24/2009
  • Status: Active Grant
First Claim
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1. The preparation method of the most plant-scale essentially pure methylene blue pentahydrate form A, whereinA) methylene blue is suspended in water content correspond in the organic solvent that water activity is at least 0.4 of 25 DEG C, by this suspensionLiquid is maintained at temperature and is 0-35 DEG C, and carries out separating and being dried by solid, thus removes organic solvent and any from solidThe water of excess;

  • B) methylene blue is dissolved at a temperature of 40-100 DEG C water content corresponding to being at least 0.4 have at the water activity of 25 DEG CIn machine solvent, this solution is cooled down, carry out separating and being dried by the solid of precipitation, thus from solid, remove organic solvent and appointThe water of what excess;

    OrC) methylene blue is dissolved in water content correspond in the organic solvent that water activity is at least 0.4 of 25 DEG C, and shouldThe water of organic solvent and any excess is evaporated to dry solid;

    The step that described methylene blue pentahydrate form A is wherein dried water and/or solvent to remove excess is passed throughDry in wet inert gas flow is carried out, and wherein drying condition makes MTC pentahydrate form A the most dehydrated;

    And the content that the most dried methylene blue pentahydrate form A has form A is based on methylene blue gross weight extremelyFew 95wt%,Wherein organic solvent selected from methanol, ethanol, 1-propanol, 2-propanol, 2-methyl-2-propanol, acetonitrile, oxolane, Isosorbide-5-Nitrae-Dioxane and their mixture,Wherein the water content of liquid phase be less than 50wt%, gross weight based on this liquid phase, andA) drying condition and b) is the phase using the inert gas flow temperature at not higher than 40 DEG C with the gas being not less than 30%Carry out under humidity, and c) in evaporation enter under the relative humidity of the temperature of not higher than 40 DEG C and the gas that is not less than 30%OK.

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