Method for synthesizing pentafluorophenol by using microchannel reactors

A technology of microchannel reactor and pentafluorophenol, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of long reaction cycle, complicated operation, high energy consumption, etc., achieve short reaction time, The operation process is simple and the effect of reducing side reactions

Active Publication Date: 2015-07-15
RUICHENG COUNTY SIPULUNDI BIOLOGICAL ENG CO LTD
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  • Abstract
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  • Claims
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Problems solved by technology

Its disadvantage is that the above synthetic methods are all completed through the operation of the tank reactor, the reaction cycle is long, the operation is complicated, the energy consumption is large, and the cost is high

Method used

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  • Method for synthesizing pentafluorophenol by using microchannel reactors

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] (1) Three microchannel reactors are connected in series; the microchannel reactors are replaced with nitrogen.

[0019] (2) Weigh 100g of pentafluorobromobenzene and dissolve it in 786.5ml (about 700g) of tetrahydrofuran to form a homogeneous solution with a volume of about 840ml; weigh 230ml of 2mol / L n-butyllithium n-hexane solution;

[0020] (3) Control the flow rate of pentafluorobromobenzene tetrahydrofuran mixture to 60ml / min; control the flow rate of n-butyllithium n-hexane solution to 16ml / min; two streams of materials flow through reactor Ⅰ in the microchannel reactor at the same time; The time is 10s, and the reaction temperature is -40°C;

[0021] (4) Weigh 104g of trimethyl borate, with a volume of about 114ml; control the flow rate of trimethyl borate to be 7ml / min, and flow through the microchannel reactor simultaneously with the output of reactor I (flow rate of about 70ml / min). Reactor Ⅱ; The reaction residence time is 8s, and the reaction temperature i...

Embodiment 2

[0026] Step (1): the microchannel reactor is replaced with nitrogen;

[0027] Step (2): Weigh 100g of pentafluorobromobenzene and dissolve it in 786.5ml (about 700g) of tetrahydrofuran to form a homogeneous solution with a volume of about 840ml;

[0028] Step (3): Measure 230ml of 2mol / L n-butyllithium n-hexane solution; control the flow rate of pentafluorobromobenzene tetrahydrofuran mixture to 60ml / min; control the flow rate of n-butyllithium n-hexane solution to 16ml / min; The materials flow through the reactor I in the microchannel reactor at the same time; the reaction residence time is 10s, and the reaction temperature is -30°C;

[0029] Step (4): Weigh 104g of trimethyl borate, with a volume of about 114ml; control the flow rate of trimethyl borate to 7ml / min, and flow simultaneously with the discharge of reactor I in step (3) (flow rate of about 70ml / min) Through reactor II in the microchannel reactor; the reaction residence time is 8s, and the reaction temperature is ...

Embodiment 3

[0034] Step (1): the microchannel reactor is replaced with nitrogen;

[0035] Step (2): Weigh 100g of pentafluorobromobenzene and dissolve it in 786.5ml (about 700g) of tetrahydrofuran to form a homogeneous solution with a volume of about 840ml; weigh 230ml of 2mol / L n-butyllithium n-hexane solution;

[0036] Step (3): Control the flow rate of pentafluorobromobenzenetetrahydrofuran mixed solution to be 60ml / min; control the flow rate of n-butyllithium n-hexane solution to be 16ml / min; two streams of materials flow through reactor I in the microchannel reactor simultaneously; The reaction residence time is 10s, and the reaction temperature is -20°C;

[0037] Step (4): Weigh 104g of trimethyl borate, with a volume of about 114ml; control the flow rate of trimethyl borate to 7ml / min, and flow simultaneously with the discharge of reactor I in step (3) (flow rate of about 70ml / min) Through the reactor II in the microchannel reactor; the reaction residence time is 8s, and the react...

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Abstract

The invention relates to a method for synthesizing pentafluorophenol by using microchannel reactors, which has the advantages of high reaction speed, short production cycle, low cost and high product purity. The method comprises the following steps: connecting three microchannel reactors in series, and dissolving pentafluorobromobenzene in an ether solvent to obtain a homogeneous mixed solution; respectively pumping the homogeneous mixed solution and an n-butyllithium n-hexane solution into a reactor I to react, thereby obtaining a reaction solution I; respectively pumping borate and the reaction solution I in a volume flow ratio of 1:(5-15) into a reactor II to react, thereby obtaining a reaction solution II; adding dilute hydrochloric acid into the reaction solution II for neutralization until the pH value is 1-3, standing, carrying out oil-water separation, and obtaining a pentafluorobenzene boric acid solution in the oil phase; pumping a 30 mol% oxydol solution and the pentafluorobenzene boric acid solution in a volume flow ratio of 1:(0.5-5) into a reactor III, and reacting to obtain a pentafluorophenol crude product solution; adding a 10 wt% sodium sulfite solution, removing excessive oxydol, washing with water, drying, and rectifying under vacuum to obtain the pentafluorophenol.

Description

technical field [0001] The invention relates to a method for synthesizing pentafluorophenol with a microchannel reactor, belonging to the technical field of organic synthesis. Background technique [0002] Pentafluorophenol is the abbreviation of 2,3,4,5,6-pentafluorophenol, an important fine chemical intermediate, mainly used in the preparation of high-performance OLED display materials, sofosbuvir medicine, plant growth regulation Agents can also be used for peptide synthesis. Its market demand is increasing, and the quality requirements are getting higher and higher. Therefore, the research on the synthesis method of pentafluorophenol has practical significance. At present, the synthesis methods of pentafluorophenol mainly include: the Grignard reagent method disclosed in Chinese Patent Document 1 (CN103420801A), the high-pressure catalytic hydrolysis and acidification method disclosed in Chinese Patent Document 2 (CN 102887817A); One-pot method of lith...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/27C07C37/01
Inventor 张彦军冯中铎肖超郭斌孙军
Owner RUICHENG COUNTY SIPULUNDI BIOLOGICAL ENG CO LTD
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