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A new crystal form of oxoethylamine compound
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A technology of compounds and crystal forms, applied in the field of medicinal chemistry, can solve the problems of deliquescence, inability to realize industrial production, etc., and achieve the effect of simple purification
Active Publication Date: 2022-03-04
ZENJI RES LAB
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CN111386276A discloses a method for preparing substituted polycyclic pyridone derivatives, which involves an intermediate formula (I) compound, and studies whether the phosphate, benzoic acid, hydrochloric acid, sulfate, etc. of the formula (I) compound are in a crystalline state, wherein Phosphate, methanesulfonate, and p-chlorobenzoate are in crystalline state, but the crystals of methanesulfonate and p-chlorobenzoate will deliquesce in the air, and industrial production cannot be realized. Only phosphate will not deliquesce ,
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Embodiment 1
[0024] Embodiment 1: the screening of salt
[0025] Method: Take 1g of the compound of formula (1) in 3ml of methyl tetrahydrofuran, add 1 equivalent of acid, stir at room temperature and observe whether a solid is precipitated (temperature: 15°C).
[0026]
[0027] During the salt-forming process of 11 acids, only phosphoric acid, fumaric acid, L-tartaric acid and succinic acid appeared solid. However, L-tartaric acid and succinic acid absorb moisture significantly during suction filtration, and phosphate and fumarate have better solid state. Observed under an optical microscope, the crystal habit collection of phosphate and fumarate solids are shown in the appendix respectively. figure 2 , 3 .
[0028] Comparison of solid suction filtration time of phosphate and fumarate:
[0029]
[0030] Phosphate will lead to prolonged suction filtration time, which is not conducive to industrial scale-up production.
[0031] The fumarate solid of the compound of formula (1) i...
Embodiment 2
[0036] Repeat CN111574386 embodiment 6
[0037] Add 20.2 g of potassium hydroxide and 24.5 g of ethanolamine into a 1000 ml four-necked flask, raise the temperature to 100° C., add 10.0 g of 2-chloroacetaldehyde dimethyl acetal, and keep the reaction for 10 hours. Cool down to room temperature, add 70ml of water-soluble clear, after cooling down to room temperature, extract with dichloromethane for later use, add 2.02g of oxalic acid, stir and add 0.05g of oxalate seed crystals, keep warm at 0°C and stir for 2h, filter, gelatinous It takes 1h to dry.
Embodiment 3
[0039] Take 1 g of the compound of formula (1) in 5 ml of dichloromethane, add 0.39 g of fumaric acid, precipitate a solid, and filter it with suction to obtain 1.20 g. After XRD detection, the solid is fumarate crystal form I, and its crystal habit map is attached image 3 .
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Abstract
The invention relates to a new crystal form of an intermediate for preparing tricyclic pyridine derivatives, in particular to a new crystal form of fumarate of an oxoethylamine compound. Specifically, the present invention provides a fumarate crystal form I of the compound of formula (I). The crystal form I has a good crystal habit and is suitable for industrial production.
Description
technical field [0001] The invention belongs to the field of medicinal chemistry, and relates to a new crystal form of an intermediate for preparing tricyclic pyridine derivatives, in particular to a new crystal form of fumarate of an oxoethylamine compound. Background technique [0002] Tricyclic pyridine derivatives such as 7-hydroxy-3,4,12,12a-tetrahydro-1H-[1,4]azino[3,4-c]pyrido[2,1-f][1,2 ,4] Triazine-6,8-dione is used as the core backbone of substituted polycyclic pyridone derivatives with cap-dependent endonuclease inhibitory activity and as a shared backbone for other compounds with Drugs such as those compounds having HIV integrase inhibitory activity. CN111386276A discloses a method for preparing substituted polycyclic pyridone derivatives, which involves an intermediate formula (I) compound, and studies whether the phosphate, benzoic acid, hydrochloric acid, sulfate, etc. of the formula (I) compound are in a crystalline state, wherein Phosphate, methanesulfonat...
Claims
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