Crystal forms of camostat mesylate and solvate thereof as well as preparation method and application of crystal forms of camostat mesylate and solvate thereof
A technology of ester mesylate and crystal form, which is applied in the preparation of organic compounds, sulfonate preparation, chemical instruments and methods, etc., and can solve problems such as unfavorable drug stability
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Embodiment 1
[0083] The preparation of embodiment 1 hydrate crystal form C
[0084]Add 5g of the free base to 25ml of deionized water, cool down to 10-15°C, add dropwise a methanesulfonic acid solution prepared by 1.2g methanesulfonic acid and 1.5g water, and keep the temperature not exceeding 20°C during the dropping process. After dropping, the system was dissolved and cleared, cooled to 0-5°C and stirred for 2 hours, and a solid was precipitated. Filter, rinse the filter cake with cold water, and blow dry at 50°C for 6h to obtain 3.1g of the compound of formula (I) 4-(4-guanidinobenzoyloxy)phenylacetic acid [2-(dimethylamino)-2 Hydrate form C of -oxoethyl] ester methanesulfonate.
Embodiment 2
[0085] The preparation of embodiment 2 acetone solvate crystal form E
[0086] 5 g of the free base was added to a mixture of 45 ml of acetone and 5 ml of deionized water, and a suspension was obtained under stirring. At 15-25°C, add dropwise a methanesulfonic acid solution prepared by 1.2g methanesulfonic acid and 2.4g water, and keep the temperature not exceeding 25°C during the dropping process. After dropping, the system dissolves and clears. The temperature was lowered to -10~0°C, and a solid was precipitated. Insulated and stirred for 2h, filtered, the filter cake was rinsed with acetone, and dried at 50°C for 4h to obtain 3.8g of formula (I) compound 4-(4-guanidinobenzoyloxy)phenylacetic acid [2-(dimethyl Acetonide form E of amino)-2-oxoethyl] ester mesylate.
Embodiment 3
[0087] Example 3 Preparation of N,N-dimethylformamide solvate crystal form F
[0088] 5 g of the free base was added to 15 ml of N,N-dimethylformamide, and a suspension was obtained under stirring. At 15-25°C, add 1.2g of methanesulfonic acid dropwise, and keep the temperature not exceeding 25°C during the dropwise addition. After dropping, the system dissolves and clears. The temperature was lowered to 0-5°C, and a solid was precipitated. Keep stirring for 2 hours, filter, rinse the filter cake with frozen N,N-dimethylformamide, and air-dry at 90°C for 5 hours to obtain 3.3g of compound 4-(4-guanidinobenzoyloxy) of formula (I) ) N,N-dimethylformamide solvate crystal form F of [2-(dimethylamino)-2-oxoethyl] phenylacetate methanesulfonate.
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