Eplerenone solvate and preparation method thereof
A technology of eplerenone and solvate, applied in the field of pharmaceutical preparation, can solve the problems of failing to meet pharmacopoeia standards, large loss of raw materials and solvents, large solvent residues, etc., and achieves good impurity removal effect, small solvent residues, The effect of improving purity
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Embodiment 1
[0039] According to Example 26 (page 139) of patent EP1223174, the oxidation reaction is completed, and the reaction solution is washed and concentrated to dryness to obtain a primary synthetic product of eplerenone with a purity of 86.12%.
[0040] A preparation method of eplerenone solvate, comprising the steps of: adding 500 g of the primary synthetic eplerenone into 5 L of 1,4-dioxane, heating to 90° C., stirring for 0.5 h, and cooling to 0°C, filter, and dry the filter cake at 80°C for 3 hours to obtain 510 g of eplerenone solvate containing 16.83% 1,4-dioxane, with a yield of 84.8% and a purity of 98.77%.
[0041] A preparation method for L crystal form eplerenone, comprising the following steps: drying 500 g of 1,4-dioxane solvate at 100° C. for 6 hours to obtain 415.5 g of L crystal form eplerenone with a purity of 98.77 %.
Embodiment 2
[0043] According to Example 26 (page 139) of patent EP1223174, the oxidation reaction is completed, and the reaction solution is washed and concentrated to dryness to obtain a primary synthetic product of eplerenone with a purity of 85.27%.
[0044] A preparation method of eplerenone solvate, comprising the steps of: adding 50 g of eplerenone primary synthetic product to 750 ml of water / 1,4-dioxane (3 / 10, v / v) mixed solvent , heated to 60°C, stirred for 2 hours, cooled to 20°C, stirred and crystallized for 2 hours, filtered, and the filter cake was dried under reduced pressure at 40°C for 6 hours to obtain eplerenone containing 15.47% 1,4-dioxane The solvate was 50g, the yield was 84.5.0%, and the purity was 98.45%.
[0045] A preparation method of L crystal form eplerenone, comprising the following steps: drying 45 g of 1,4-dioxane solvate at 95° C. for 4 hours under reduced pressure to obtain 38 g of L crystal form eplerenone, with a purity of is 98.45%.
Embodiment 3
[0047] According to Example 26 (page 139) of patent EP1223174, the oxidation reaction is completed, and the reaction solution is washed and concentrated to dryness to obtain a primary synthetic product of eplerenone with a purity of 85.58%.
[0048]A preparation method of eplerenone solvate, comprising the steps of: adding 500 g of eplerenone primary synthetic product to 4L of ethanol / 1,4-dioxane (1 / 10, v / v) and mixing In a solvent, heat to 75°C, stir for 1h, cool down to 10°C, stir and crystallize for 1h, filter, and dry the filter cake at 60°C for 4h under reduced pressure to obtain Epril containing 14.55% 1,4-dioxane Ketone solvate 502.5g, yield 85.9%, purity 98.54%. .
[0049] A preparation method of L crystal form eplerenone, comprising the following steps: drying 500 g of 1,4-dioxane solvate at 100° C. for 3 hours under reduced pressure to obtain 422.2 g of L crystal form eplerenone, 98.54% purity.
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