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Combined reactor and method of preparing pyrazolyl benzaldehyde acetal p-phenylene diamine bis-schiff base by using combined reactor

A combined reactor, double Schiff base technology, applied in chemical instruments and methods, chemical/physical/physical-chemical reactors, instruments, etc., can solve problems such as insufficient reaction, achieve rapid cooling, rapid air cooling, and improve The effect of efficiency and yield

Active Publication Date: 2017-07-21
陈宗源
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention aims at many deficiencies in the prior art, and provides a combined reactor and a method for preparing pyrazolylbenzaldehyde p-phenylenediamine bis-Schiff base using the combined reactor. The reactor mainly includes There is a heating magnetic stirrer with a vacuum chamber that can accurately control the temperature and a supporting reaction device. With this device, the temperature can be precisely controlled and the problems of local overreaction, insufficient reaction, and liquid splash in the traditional Schiff base synthesis process can be overcome. At the same time, it is disclosed A method for preparing pyrazolylbenzaldehyde acetal p-phenylenediamine bis-Schiff base with the reactor is proposed, and the obtained bis-Schiff base has a larger conjugated π structure, which improves the efficiency of the reaction and saves the reaction time

Method used

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  • Combined reactor and method of preparing pyrazolyl benzaldehyde acetal p-phenylene diamine bis-schiff base by using combined reactor
  • Combined reactor and method of preparing pyrazolyl benzaldehyde acetal p-phenylene diamine bis-schiff base by using combined reactor
  • Combined reactor and method of preparing pyrazolyl benzaldehyde acetal p-phenylene diamine bis-schiff base by using combined reactor

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Effect test

Embodiment 1

[0046] A combined reactor, comprising a magnetic stirrer capable of precise temperature control and a reactor placed in the magnetic stirrer, the reactor is a three-necked flask, the flask is equipped with a dropping funnel, the dropping funnel Installed with slow flow connector;

[0047] Among them such as Figure 1-6 As shown, the magnetic stirrer that can precisely control the temperature includes a base 1-1 and an oil bath 1-7 arranged on the base 1-1, and the outside of the oil bath 1-7 is provided with a vacuum chamber 1- 3, and the oil bath 1-7 is provided with a control system;

[0048] The vacuum chamber 1-3 is provided with two vacuum ports 1-2;

[0049] The control system includes a temperature control switch 1-4, a speed switch 1-5 and a display screen 1-6, the temperature of the oil bath is controlled by the temperature control switch 1-4, and the speed of magnetic stirring is controlled by the speed switch 1-5. The oil bath is provided with corresponding elect...

Embodiment 2

[0056] Utilize the combined reactor described in embodiment 1 to prepare the method for pyrazolylbenzaldehyde acetal p-phenylenediamine bis-Schiff base, concrete steps are as follows:

[0057] Weigh 0.57g (8.4mmol) of pyrazole, 2.32g (16.8mmol) of potassium carbonate, dissolve in 18.974g (259.6mmol) of N,N-dimethylformamide, add to the oven equipped with rotor, thermometer and In the 100mL three-necked flask of the dropping funnel of the slow-flow joint, react at 100°C for 30min under constant temperature stirring, and dropwise add p-fluorobenzaldehyde 1.04g (8.4mmol) to the mixed solution through the dropping funnel with the slow-flow joint, Continue the reaction for 10 hours, pass cold air into the vacuum chamber through two vacuum ports, and quickly cool the oil bath to room temperature to obtain the crude pyrazolylbenzaldehyde, recrystallize with absolute ethanol, and vacuum-dry at 50°C for 8 hours. That is, pyrazolylbenzaldehyde.

[0058] Weigh 0.11g (0.65mmol) of pyrazo...

Embodiment 3

[0060] Utilize the combined reactor described in embodiment 1 to prepare the method for pyrazolylbenzaldehyde acetal p-phenylenediamine bis-Schiff base, concrete steps are as follows:

[0061] Weigh 1.36g (20mmol) of pyrazole and 5.53g (40mmol) of potassium carbonate, dissolve them in 37.95g (519.2mmol) of N,N-dimethylformamide, and add them to a furnace equipped with a rotor, a thermometer and a device with slow flow. In the 100mL three-necked flask of the dropping funnel of the connector; after reacting for 30min under constant temperature stirring at 110°C, add 2.482g (20mmol) of p-fluorobenzaldehyde dropwise to the mixed solution through the dropping funnel with a slow flow connector, and continue the reaction After 12 hours, use a vacuum chamber to quickly cool to room temperature to obtain the crude product, recrystallize it with absolute ethanol, and dry it in vacuum at 50°C for 8 hours to obtain pyrazolylbenzaldehyde.

[0062] Weigh 0.172g (1mmol) of pyrazolylbenzaldeh...

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Abstract

The invention relates to a combined reactor and a method of preparing pyrazolyl benzaldehyde acetal p-phenylene diamine bis-schiff base by using the combined reactor. The reactor mainly comprises a heating magnetic stirrer and a mating reaction device, wherein the heating magnetic stirrer is provided with a vacuum chamber and can conduct accurate temperature control. The reactor can conduct the accurate temperature control and overcome the problems of local over excitation reaction, insufficient reaction, liquid splash and the like in the traditional schiff base synthesis process. At the same time, the invention discloses the method of preparing pyrazolyl benzaldehyde acetal p-phenylene diamine bis-schiff base by using the reactor. Prepared bis-schiff base has a greater conjugated pi structure; the reaction efficiency is improved; and the reaction time is saved.

Description

technical field [0001] The invention relates to the fields of chemical experiment equipment and chemical synthesis, in particular to a combined reactor and a method for preparing pyrazolylbenzaldehyde p-phenylenediamine bis-Schiff base using the combined reactor. Background technique [0002] Schiff base mainly refers to a class of organic compounds containing imine or methylimine characteristic group (-RC=N-), which has a special conjugated structure and good chemical coordination performance, and some of its metal complexes have good It has been used as a fluorescent probe to identify metal ions due to its unique fluorescence properties, which has aroused people's more in-depth theoretical and synthetic application research. [0003] Most of the Schiff base synthesis needs to be reacted in a closed system. Generally, a multi-necked flask is used as a reaction vessel, and the middle opening of a conventional multi-necked flask is equipped with a stirrer, while other ports a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D231/12C09K11/06G01N21/64B01F13/08B01J19/00B01L7/02
CPCB01J19/0093G01N21/6402C09K11/06C07D231/12B01L7/02C09K2211/1044C09K2211/1007B01F33/452
Inventor 陈宗源秦大伟王樊伟
Owner 陈宗源
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