A kind of crystal form of quinazoline compound and preparation method thereof
A technology of quinazolines and compounds, which is applied in the field of crystal forms of quinazolines and their preparation, can solve problems such as excessive cell proliferation, and achieve the effects of simple and easy-to-operate preparation methods, safe clinical medication, and good stability
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Embodiment 1
[0122] This embodiment is the preparation method of quinazoline compound crystal form A described in the present invention, comprising the following steps:
[0123] (1) The crude product 3.00g of quinazoline compound is washed 2 times with purified water (4.65g), ethanol (1.90g), after controlling vacuum-0.08MPa temperature 20 ℃ of drying 2 hours in vacuum oven, then heat up Dry at 50°C for 20 hours, take out the solid, then add 38.0g of dimethyl sulfoxide (DMSO) to 40°C and stir to dissolve, filter, add purified water (70g) and stir, and then filter;
[0124] (2) The quinazoline compounds that have completed step (1) are washed sequentially with 7.0 g of purified water and 3.8 g of ethanol, then heated to 78°C with 37.0g of ethanol for beating under reflux for 3 hours, cooled to 20°C for filtration, and then After washing with 3.70g of ethanol, add 27g of absolute ethanol, then add 7.80g of dimethyl sulfoxide (DMSO), heat at 78°C, continue stirring for 3h, drop to 20°C and fi...
Embodiment 2
[0127] This embodiment is the preparation method of quinazoline compound crystal form A described in the present invention, comprising the following steps:
[0128] (1) 3.00 g of the crude product of quinazoline compounds are washed twice with purified water (4.65 g), ethanol (1.90 g), and after drying for 2 hours at a temperature of 30° C. of vacuum-0.10 MPa in a vacuum oven, the temperature is raised Dry at 55°C for 20 hours, take out the solid, then add 38.0g of dimethyl sulfoxide (DMSO) to 45°C and stir to dissolve, filter, add purified water (70g) and stir, and then filter;
[0129] (2) The quinazoline compounds that have completed step (1) are washed sequentially with 7.0 g of purified water and 3.8 g of ethanol, then heated to 70°C with 37.0g of ethanol to reflux for beating for 2 hours, cooled to 20°C for filtration, and then After washing with 3.70g of ethanol, add 27g of absolute ethanol, then add 7.80g of dimethyl sulfoxide (DMSO), heat at 83°C, continue to stir for...
Embodiment 3
[0132] This embodiment is the preparation method of quinazoline compound crystal form A described in the present invention, comprising the following steps:
[0133] (1) The crude product 3.00g of quinazoline compound is washed 2 times with purified water (4.65g), ethanol (1.90g), after controlling vacuum-0.09MPa temperature 20 ± 10 ℃ of drying 2 hours in vacuum oven, Then raise the temperature to 45°C and dry for 20 hours, take out the solid, then add 38.0 g of dimethyl sulfoxide (DMSO) and stir to dissolve at 35°C, filter, add purified water (70 g) and stir, and then filter;
[0134] (2) The quinazoline compounds that have completed step (1) are washed sequentially with 7.0 g of purified water and 3.8 g of ethanol, then heated to 80° C. for reflux with 37.0 g of ethanol for beating for 5 hours, cooled to 20° C., filtered, and then After washing with 3.70g of ethanol, add 27g of absolute ethanol, then add 7.80g of dimethyl sulfoxide (DMSO), heat at 72°C, continue stirring for ...
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