Complex and preparation method thereof, preparation method of polybutadiene
A complex, butadiene technology, applied in iron organic compounds, chemical instruments and methods, compounds containing elements of Group 6/16 of the periodic table, etc., can solve the problems of low selectivity, low high temperature activity, air sensitivity, etc.
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[0042] The present invention also provides a preparation method for the complex of the above formula (I), comprising the following steps: A) mixing the compound of the formula (II), the alkali metal hydride and the compound of the formula (III) in the first organic solvent The reaction is carried out by heating in medium to obtain the compound of formula (IV);
[0043] B) reacting the compound of formula (IV) with the tetrahydrofuran complex of metal chloride in a second organic solvent to obtain the complex of formula (I); the metal chloride is iron chloride or Chromium chloride;
[0044]
[0045] Among them, R 1 with R 2 Each is independently hydrogen, C1-C10 alkyl, phenyl or substituted phenyl, preferably hydrogen, methyl, isopropyl, phenyl or p-chlorophenyl; M is Fe or Cr; n is 2 or 3 ; X is a halogen, preferably Cl or Br, more preferably Cl.
[0046] All raw materials in the present invention have no special limitation on their sources, and they can be commercially...
Embodiment 1
[0063] 1.1 Under nitrogen protection, add 0.12g (50mmol) sodium hydride to a stirred 50ml dimethylformamide (DMF) solution containing 0.34g (50mmol) pyrazole, stir for a few minutes, then slowly add 1.07g ( 50mmol) 2-chloro-1,10-phenanthroline, reflux for 72h, cool, add cold water, filter out the white precipitate, and recrystallize with ethanol to obtain white crystal 2-pyrazole-1,10-phenanthroline , and the yield was 82.1%. The above reaction process is as follows:
[0064]
[0065] 1.2 Under the condition of nitrogen protection, add 0.24g (1.2mmol) FeCl2 4H2O to the 15ml tetrahydrofuran solution containing 0.30g (1.2mmol) 2-pyrazole-1,10-phenanthroline prepared in 1.1, Stir the reaction at room temperature for 6 h, add diethyl ether to the reaction system to produce a red suspension, filter, wash the filtrate three times with diethyl ether and heptane successively, and vacuum-dry to obtain red solid complex 1 with a yield of 85.6%. The reaction process is as follows: ...
Embodiment 2
[0071] 2.1 Under nitrogen protection, add 0.12g (50mmol) sodium hydride to a stirred 50ml dimethylformamide (DMF) solution containing 0.48g (50mmol) 3,5-dimethylpyrazole, and stir for a few minutes , then slowly add 1.07g (50mmol) 2-chloro-1,10-phenanthroline, reflux for 72h, cool down, add cold water, filter out the white precipitate, and recrystallize with ethanol to obtain white crystal 2-(3, 5-dimethylpyrazole)-1,10-phenanthroline with a yield of 81.8%. The above reaction process is as follows:
[0072]
[0073] 2.2 Under the condition of nitrogen protection, add 0.22g (1.1mmol) FeCl2 4H2O to 0.30g (1.1mmol) 2-(3,5-dimethylpyrazole)-1,10- In 15ml tetrahydrofuran solution of phenanthroline, stir and react at room temperature for 6h, add diethyl ether to the reaction system to produce a red suspension, filter, wash the filtrate three times with diethyl ether and heptane successively, and vacuum dry to obtain a red solid compound Material 7 with a yield of 91.8%. The re...
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