Crystalline pharmaceutical co-crystals of glycopyrronium bromide with lactose
A technology of glycopyrronium bromide and lactose, which is applied in the field of co-crystallization of glycopyrronium bromide and lactose, can solve the problem of short time, such as 0.6 to 1.2 hours
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Embodiment 1
[0113] Example 1-Preparation of the co-crystal of glycopyrrolate and lactose
[0114] Glycopyrrolate (2.0 g; 5.0 mmol) and lactose monohydrate (1.98 g; 5.49 mmol) were dissolved in dimethyl sulfoxide (DMSO) (10 ml) at a temperature of 50°C to 55°C. Then, while keeping the reaction mixture at a temperature of 50°C to 55°C, ethyl acetate (50 ml) was added dropwise.
[0115] A suspension is obtained, and the reaction mixture is cooled to a temperature of 20 to 25°C and kept at this temperature with stirring for 3 hours.
[0116] The product was filtered and washed with ethyl acetate, and then dried in vacuum at a temperature of 35°C to 40°C to obtain 3.7 g of a co-crystal of glycopyrrolate and lactose.
[0117] The product was analyzed using differential scanning calorimetry (DSC). XRPD results showed that a new crystal form was formed: a co-crystal of glycopyrrolate and lactose.
[0118] The XRPD and DSC of the eutectic are characterized in figure 1 with 2 Described as'GBr1' in.
Embodiment 2
[0119] Example 2-Preparation of co-crystal of glycopyrrolate and lactose
[0120] Glycopyrrolate (2.0 g; 5.0 mmol) and lactose monohydrate (1.98 g; 5.49 mmol) were dissolved in dimethylformamide (DMF) (10 ml) at a temperature of 50°C to 55°C. Then, while keeping the reaction mixture at a temperature of 50°C to 55°C, ethyl acetate (50 ml) was added dropwise.
[0121] A suspension was obtained, and the reaction mixture was cooled to a temperature of 20 to 25°C and kept at this temperature with stirring for 3 hours.
[0122] The product was filtered and washed with ethyl acetate, and then dried under vacuum at a temperature of 35°C to 40°C to obtain 3.83 g of a co-crystal of glycopyrrolate and lactose.
[0123] The product was analyzed using differential scanning calorimetry (DSC). XRPD results showed that a new crystal form was formed: a co-crystal of glycopyrrolate and lactose.
[0124] The XRPD and DSC of the eutectic are characterized in figure 1 with 2 It is described as'GBr2'.
Embodiment 3
[0125] Example 3 Preparation of co-crystal of glycopyrrolate and lactose
[0126] Glycopyrrolate (2.0 g; 5.0 mmol) and lactose monohydrate (1.98 g; 5.49 mmol) were dissolved in dimethylformamide (DMF) (40 ml) at a temperature of 50°C to 55°C. Then, while keeping the reaction mixture at a temperature of 50°C to 55°C, methyl ethyl ketone (MEK) (80 ml) was added dropwise.
[0127] A suspension is obtained, and the reaction mixture is cooled to a temperature of 20 to 25°C and kept at this temperature with stirring for 3 hours.
[0128] The product was filtered, washed with methyl ethyl ketone (MEK), and then dried in vacuum at a temperature of 35°C to 40°C to obtain 3.06 g of a co-crystal of glycopyrrolate and lactose.
[0129] The product was analyzed using differential scanning calorimetry (DSC). XRPD results showed that a new crystal form was formed: a co-crystal of glycopyrrolate and lactose.
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