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[ CAS No. 50849-45-1 ] {[proInfo.proName]}

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Chemical Structure| 50849-45-1
Chemical Structure| 50849-45-1
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CAS No. :50849-45-1 MDL No. :MFCD02114464
Formula : C48H38N4 Boiling Point : -
Linear Structure Formula :- InChI Key :-
M.W : 670.86 Pubchem ID :-
Synonyms :

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Application In Synthesis of [ 50849-45-1 ]

* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.

  • Downstream synthetic route of [ 50849-45-1 ]

[ 50849-45-1 ] Synthesis Path-Downstream   1~1

  • 1
  • [ 109-97-7 ]
  • [ 620-23-5 ]
  • [ 50849-45-1 ]
YieldReaction ConditionsOperation in experiment
53%
46% With butyric acid In N,N-dimethyl-formamide at 55 - 150℃; 3 Pyrrole and 3-methylbenzaldehyde in a molar ratio of 1: 1.1 were dissolved in DMF solvent, then add butyric acid to obtain a mixed solution, among them, Butyric acid and DMF mass ratio of 50:50, pyrrole and 3-methylbenzaldehyde accounted for 10% of the total mass of butyric acid and DMF, The mixed solution from the constant temperature sedimentation tower inlet of the reaction material was added to the reaction separation synchronous reactor, Until it is filled with the reaction zone of the constant temperature sedimentation tower and the stirring reaction tower, By heating the jacket to control the temperature in the stirring reaction tower at 150 °C , turn on the stirrer to stir the reaction, At the same time control the temperature of the constant temperature tower at 55 °C , and open the circulating pump control the amount of circulation per hour for the mixed raw material volume of 25% The reaction continued, Porphyrin products containing methyl substituents are continuously precipitated in a constant temperature settling tower, Subsidence in the microporous filter plate, until the reaction is carried out until no precipitate precipitates in the constant temperature settling tower, Stop the reaction, the remaining reaction solution discharged from the liquid outlet recovery, add the new pyrrole and 3-methylbenzaldehyde for the next pot reaction, from the thermostatic settling tower to obtain a methyl group containing porphyrin product, Recrystallization by DMF and drying gave porphyrin products with a purity of more than 99%. The yield was 46%.
44.6% Stage #1: pyrrole; m-tolyl aldehyde In propionic acid; m-xylene at 159.6℃; for 0.25h; Large scale; Green chemistry; Stage #2: With air In propionic acid; m-xylene for 0.3h; Large scale; Green chemistry; 7 (1) 560 mol of pyrrole and 560 mol of benzaldehyde were mixed to prepare a mixed solution, alternate;(2) In a 2000L titanium high pressure polymerization reactor 1 with mechanically stirred and electrically heated jacket with distillation device on top, solvent E consisting of 840L propionic acid and 560L cyclohexane was added, and the concentration of oxygen in the gas phase from the bottom of the polymerization reactor 1 where N2 is bubbled into the top of the reactor condenser was less than 1%,then, the polymerization reactor 1 was started to heat the jacket switch, the liquid in the polymerization reactor 1 was heated to reflux, maintaining the polymerization reactor 1 pressure 5.0 atm, at the same time, the mixed solution prepared in step (1) was added dropwise from the top of the polymerization reactor 1 in a dropwise manner, and the molar concentration of pyrrole in the reaction liquid was maintained at less than 0.1 mol/L during the dropwise addition. The water produced by the reaction was removed from the system through the distillation device at the top of the polymerization reactor 1, condensed, and then separated by the liquid-liquid layering device 4, and the upper oil phase was recycled back to the reaction system. The reflux ratio of the distillation column was constantly adjusted so that the water concentration in the polymerization reactor 1 was always lower than 0.05%.After the addition, the reaction was continued at the same time, and the reaction was stopped after 15 minutes. At the end of the reaction, the reaction temperature was 157.1°C. At this point, the polymerization reactor 1 is maintained at a pressure of 5 atm, air was passed into the oxidation reaction, oxidation reaction time was 22 minutes, during the reaction, the oxygen concentration in the exhaust gas was strictly controlled to be less than 2% by adjusting the amount of passed air. After completion of the oxidation reaction, left to cool slowly. When the temperature of the liquid in the polymerization reactor 1 drops to room temperature, it was filtered through the filter washing device 2 to obtain the filtrate and filter cake, and the filtrate was subjected to rectification and dehydration in the solvent recovery column 3 of the polymerization reaction to recover the solvent,the recovered solvent is collected to be recycled back to the system for continued use, and the residue of the tower reactor is discharged out of the system. The filtered cake was repeatedly washed with hot water and filtered until the filtrate was colorless. The filter cake was then washed repeatedly with methanol and filtered until the filtered waste water was colorless. The filter cake washed with methanol was the product TPP, after vacuum drying at 80°C51.4of 98.7%. The process flow is the same as that of Embodiment 1, except that: (1) adding 350 moles of pyrrole and 522 moles of methylbenzaldehyde; (2) Solvent E is a mixture of 980L propionic acid and 420L meta-xylene (3) The reaction time in the polymerization reactor is 15 minutes and the reaction pressure is 2.0 atm. At the end of the reaction, the reaction temperature was 159.6°C. The concentration of water in the polymerization reactor is controlled to always be less than 0.12%; (4) The gas introduced into the oxidation reactor is air, the reaction time is 18 minutes, and the reaction pressure is normal pressure; According to this method, the final solid obtained was vacuum dried at 80°C to obtain product TPP26.2 kg. The product TPP had a synthesis yield of 44.6% and a purity of 98.7% based on the reactant pyridine.
44.2% Stage #1: pyrrole; m-tolyl aldehyde With propionic acid In m-xylene at 159.6℃; for 0.25h; Stage #2: In m-xylene for 0.3h; Reflux; 5.1-5.5 Example 1 General procedure: (1) Prepare 560mol of pyrrole and 560mol of benzaldehyde into a mixed solution and set aside;(2) In a 2000L high-pressure titanium polymerization reactor 1 with a mechanical stirring and electric heating jacket and a distillation device on the top, add a solvent E consisting of 840L of propionic acid and 560L of cyclohexane,From the bottom of the polymerization reactor 1, N2 is bubbled to the oxygen concentration in the gas phase of the reactor top condenser outlet to be lower than 1%, and then the electrical heating jacket switch of the polymerization reactor 1 is started to heat the liquid in the polymerization reactor 1 to reflux. , Maintaining the pressure of the polymerization reactor 1 at 5.0atm, while adding the mixed solution prepared in step (1) from the top of the polymerization reactor 1 by dropwise addition, the molar concentration of pyrrole in the reaction solution is always kept lower than 0.1mol during the dropwise addition / L.The water produced by the reaction is removed from the system through a distillation device at the top of the polymerization reactor, and after condensing, it is delaminated by a liquid-liquid layering device 8 to circulate the upper oil phase back into the reaction system. The reflux ratio of the distillation column was continuously adjusted so that the water concentration in the polymerization reactor 1 was always lower than 0.05%. After the dropwise addition, the reaction was continued at the same time, and the reaction was stopped after 15 minutes. At the end of the reaction, the reaction temperature was 157.1 ° C. Then slowly cool it down. When the temperature in the polymerization reactor 1 drops to normal temperature, the reactants in the polymerization reactor 1 are filtered through the filtering and washing device 2 to obtain a filtrate and a crude TPP filter cake. The mass of the crude TPP filter cake is 54.8 kg. According to gas chromatography analysis, the amount of pyrrole remaining in the polymerization reaction system was 55.2 mol. The filtrate can be distilled into the polymerization solvent recovery tank 3 for distillation, and the solvent and unreacted pyrrole can be recovered. The recovered solvent and pyrrole are collected for recycling to the polymerization reactor 1 and continued to be used. The residue of the distillation kettle is discharged outside the system. deal with.(3) Add 54.8 kg of crude TPP filter cake obtained by centrifugal filtration to a 2000L oxidation reactor 4 with mechanical stirring and electric heating jacket, with condensation reflux at the top and gas distributor at the bottom, and simultaneously add 1400 kg of propylene into the kettle Acid, and simultaneously introducing nitrogen gas to replace the gas phase space in the oxidation reactor 4 to a tail oxygen concentration of less than 3%. Then, the switch of the electric heating jacket is started to heat the liquid in the oxidation reactor 4. When the liquid in the oxidation reactor 4 is heated to reflux, air is passed through to carry out the oxidation reaction. The oxidation reaction time is 22 minutes. During the reaction, the oxygen concentration in the tail gas is strictly controlled by adjusting the amount of the air to be passed to less than 3%. After the oxidation reaction was completed, it was left to cool slowly. When the temperature of the liquid in the oxidation reactor 4 is reduced to normal temperature, it is put into a filtering and washing device 5 for filtration to obtain a filtrate and a solid. The filtrate is dehydrated through an oxidation reaction solvent recovery tower 6 and dehydrated and recovered to obtain propionic acid, and the recovered propionic acid is collected. After that, it is ready to be used in the recycle and oxidation reactor 4 and the residue of the tower kettle is discharged out of the system. The filtrate can also be directly recycled to the oxidation reactor 4 without any treatment and continued to be used. The solid obtained by filtration was repeatedly washed with hot water and then filtered until the filtrate was colorless. Then repeatedly wash with methanol and then filter until the filtered wastewater is freecolor. The solid washed with methanol is the product TPP, and 46.0 kg of a tetraphenylporphine product is obtained after drying in a drying device 7 under vacuum at 80 ° C.The yield of the product TPP based on the pyrrole of the reactant was 59.3%, and the purity was 99.2%.
30% With air; chloroacetic acid In xylene for 1.5h; Heating;
With trifluoroacetic acid In xylene for 1.5h; Heating;

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