15 crown 5 and moo 2 cl 2 (h 2 o) 2 Molybdenum compounds and their preparation and application
A molybdenum compound, mocl2o2 technology, applied in the field of biomedicine, can solve problems such as the instability of ammonium tetrathiomolybdate, and achieve the effects of excellent inhibition, high yield and high purity
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Embodiment 1
[0030] Example 1 with 0.8gNa 2 MoO 4 2H 2 O was put into a 50ml round-bottomed flask containing 15ml of anhydrous methanol and 15ml of acetonitrile, placed on an electromagnetic stirrer and stirred for 30min, then slowly dripped 30% HCl, and then added 0.5ml15C5 and continued to stir for 8h to 20h. Filter and pour the filtrate into a 25ml pressure vessel. Hydrothermal synthesis at 120°C for 48h to 72h, filter to obtain a light green clear liquid, put the clear liquid in a long test tube, slowly add ether along the test tube wall to twice the height of the filtrate, seal it and let it stand, and precipitate light green after about a week Crystal, namely the compound [MoCl 2 o 2 (H 2 O) 2 ][15C5], the structure is as follows:
[0031]
[0032] Among them, MoCl 2 o 2 (H 2 O) 2 The structure of the is as follows:
[0033]
[0034] The structure of 15C5 is as follows:
[0035]
[0036] Among them, [MoCl 2 o 2 (H 2 O) 2 The crystal structure of ][15C5] is ...
Embodiment 2
[0043] Example 2 Put 1 mole of molybdenum hexacarbonyl into a 50ml round bottom flask filled with 15ml methanol and 15ml acetonitrile, place it on an electromagnetic stirrer and stir for 30min, then slowly add 30% HCl, then add 0.5ml15C5 and continue stirring 8h to 20h. Filter and pour the filtrate into a 25ml pressure vessel. Hydrothermal synthesis at 120°C for 48h to 72h, filter to obtain a light green clear liquid, put the clear liquid in a long test tube, slowly add ether along the test tube wall to twice the height of the filtrate, seal it and let it stand, and precipitate light green after about a week Crystal, namely the compound [MoCl 2 o 2 (H 2 O) 2 ][15C5], its infrared spectrum / elemental analysis and molecular and crystal structure are the same as in Example 1.
Embodiment 3
[0044] Example 3 Put 1 mole of molybdenum tetrachloride into a 50ml round bottom flask containing 15ml methanol and 15ml acetonitrile, place it on an electromagnetic stirrer and stir for 30min, then slowly add 30% HCl, then add 0.5ml15C5 and continue stirring 8h to 20h. Filter and pour the filtrate into a 25ml pressure vessel. Hydrothermal synthesis at 120°C for 48h to 72h, filter to obtain a light green clear liquid, put the clear liquid in a long test tube, slowly add ether along the test tube wall to twice the height of the filtrate, seal it and let it stand, and precipitate light green after about a week Crystal, namely the compound [MoCl 2 o 2 (H 2 O) 2 ][15C5], its infrared spectrum / elemental analysis and molecular and crystal structure are the same as in Example 1.
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