A 2-alkyl-substituted imidazolyl bisphosphonic acid compound and its preparation method and application
An acid compound and compound technology, which can be used in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, and metabolic diseases, etc., can solve the problems of low osteoclast inhibitory effect, large side effects, and high toxicity.
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Embodiment 1
[0076] The synthesis of the 2-position alkyl-substituted imidazolyl bisphosphonic acid compound with the structure represented by the formula (I) described in this example, wherein R1 is a methyl group and has the structure of the formula (II):
[0077]
[0078] The synthetic route of compound II is as follows:
[0079]
[0080] (1) Preparation of compound II intermediate 1
[0081] 8.2 g (0.1 mol) of 2-methylimidazole, 8.4 g (0.15 mol) of KOH, K 2 CO 3 13.8 g (0.1 mol) and 1.6 g (0.005 mol) of tetrabutylammonium bromide were dissolved in 75 mL of dichloromethane, and after stirring at room temperature for 0.5 h, 0.1 mol (11.2 mL) of ethyl bromoacetate was slowly added dropwise, and the dropwise addition was completed. , refluxed at 39°C for 8h, filtered, washed the filtrate three times with saturated brine, dried over anhydrous sodium sulfate, distilled the organic phase under reduced pressure at 25°C until the droplets no longer dripped, to obtain an oily substance,...
Embodiment 2
[0088] The synthesis of the 2-position alkyl-substituted imidazolyl bisphosphonic acid compound with the structure represented by the formula (I) described in this example, wherein R1 is an ethyl group and has the structure of the formula (III):
[0089]
[0090] The synthetic route of compound III is:
[0091]
[0092] (1) Preparation of compound III intermediate 1
[0093] Take 2-ethylimidazole 9.6g (0.1mol), KOH 8.4g (0.15mol), K 2 CO 3 13.8 g (0.1 mol) and 1.6 g (0.005 mol) of tetrabutylammonium bromide were dissolved in 75 mL of dichloromethane, and after stirring at room temperature for 0.5 h, 0.1 mol (11.2 mL) of ethyl bromoacetate was slowly added dropwise, and the dropwise addition was completed. , refluxed at 39°C for 8h, filtered, washed the filtrate three times with saturated brine, dried over anhydrous sodium sulfate, distilled the organic phase under reduced pressure at 25°C until the droplets no longer dripped, to obtain an oily substance, namely the co...
Embodiment 3
[0100] The synthesis of the 2-position alkyl-substituted imidazolyl bisphosphonic acid compound with the structure shown in this example, wherein R1 is a propyl group, has the structure of formula (IV):
[0101]
[0102]
[0103] The synthetic route of compound IV is:
[0104]
[0105] (1) Preparation of compound IV intermediate 1
[0106] Take 2-propylimidazole 11.0g (0.1mol), KOH 8.4g (0.15mol), K 2 CO 3 13.8 g (0.1 mol) and 1.6 g (0.005 mol) of tetrabutylammonium bromide were dissolved in 75 mL of dichloromethane, and after stirring at room temperature for 0.5 h, 0.1 mol (11.2 mL) of ethyl bromoacetate was slowly added dropwise, and the dropwise addition was completed. , refluxed at 39 °C for 9 h, filtered, washed the filtrate with saturated brine three times, dried over anhydrous sodium sulfate, distilled the organic phase under reduced pressure at 25 °C until the droplets no longer dripped, to obtain an oily substance, that is, the compound IV intermediate 1 ...
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