Imidazole heterocyclic diphosphonic acid compound as well as preparation method and application thereof
A technology of bisphosphonic acid compounds and heterocyclic compounds, applied in the field of imidazole heterocyclic bisphosphonic acid compounds and their preparation, can solve the problems of low osteoclast inhibitory effect, large side effects, and high toxicity
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Embodiment 1
[0068] The synthesis of the imidazole heterocyclic bisphosphonic acid compound having the structure shown in the formula (I) described in this example, wherein n=1, has the structure of the formula (II):
[0069]
[0070] The synthetic route of compound II is:
[0071]
[0072] (1) Preparation of Compound II Intermediate 1
[0073] Take imidazole 6.8g (0.1mol), KOH 8.4g (0.15mol), K 2 CO 3 13.8g (0.1mol) and 0.7g (7mmol) of tetrabutylammonium bromide were dissolved in 75mL of dichloromethane, and after stirring at room temperature for 0.5h, 0.1mol (11.2mL) of ethyl bromoacetate was slowly added dropwise, and the dropwise addition was completed. Reflux at 39°C for 8 hours, filter, wash the filtrate three times with saturated brine, dry over anhydrous sodium sulfate, and distill the organic phase under reduced pressure at 25°C until the liquid drops no longer drop out to obtain an oily substance, namely compound II intermediate 1;
[0074] (2) Preparation of Compound I...
Embodiment 2
[0080] The synthesis of the imidazole heterocyclic bisphosphonic acid compound having the structure shown in the formula (I) described in this example, wherein n=2, has the structure of the formula (III):
[0081]
[0082] The synthetic route of compound III is:
[0083]
[0084] (1) Preparation of Compound III Intermediate 1
[0085] Take imidazole 6.8g (0.1mol), KOH 8.4g (0.15mol), K 2 CO 3 11.1g (0.0.08mol) and tetrabutylammonium bromide 0.97g (3mmol) were dissolved in 75mL of dichloromethane, stirred at room temperature for 0.5h, slowly added dropwise ethyl bromopropionate 0.08mol (10.4mL), dropwise After completion, reflux at 50°C for 6h. Filtrate, wash the filtrate three times with saturated saline, dry over anhydrous sodium sulfate, and distill the organic phase under reduced pressure at 25°C until the liquid drops no longer drip out to obtain an oily substance, namely compound III intermediate 1;
[0086] (2) Preparation of Compound III Intermediate 2
[00...
Embodiment 3
[0092]The synthesis of the imidazole heterocyclic bisphosphonic acid compound having the structure shown in formula (I) described in this example, wherein n=3, has the structure of formula (IV):
[0093]
[0094] The synthetic route of compound IV is:
[0095]
[0096] (1) Preparation of Compound IV Intermediate 1
[0097] Take imidazole 6.8g (0.1mol), KOH 9.5g (0.17mol), K 2 CO 3 16.6g (0.12mol) and 2.3g (7mmol) of tetrabutylammonium bromide were dissolved in 75mL of dichloromethane, and after stirring at room temperature for 0.5h, 0.12mol (17.1mL) of ethyl bromobutyrate was slowly added dropwise, and the addition was completed , reflux at 30°C for 10 h, filter, wash the filtrate three times with saturated saline, dry over anhydrous sodium sulfate, and distill the organic phase under reduced pressure at 25°C until the liquid drops no longer drop out to obtain an oily substance, namely compound IV intermediate 1;
[0098] (2) Preparation of Compound IV Intermediate 2...
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