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Method for preparing 1,4-bis(difluoromethyl) tetrafluorobenzene

A technology of difluoromethyl and tetrafluorobenzene, applied in the field of preparation 1, can solve the problems of many reaction by-products, difficulty, complicated fluorination reaction equipment and the like

Inactive Publication Date: 2009-09-09
YUAN SHIN MATERIALS TECH CORP
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The disadvantages of this method are: (1) complexes of metal fluorides (such as CsF and CoF 3 ) is expensive; (2) the perfluorination reaction of hydrogen on the benzene ring and hydrogen on the branch must be carried out under high temperature (360°C); (3) this method is a gas phase reaction, so the fluorination reaction equipment is relatively Complicated; (4) There are many reaction by-products, increasing the difficulty of separation and purification

Method used

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  • Method for preparing 1,4-bis(difluoromethyl) tetrafluorobenzene
  • Method for preparing 1,4-bis(difluoromethyl) tetrafluorobenzene
  • Method for preparing 1,4-bis(difluoromethyl) tetrafluorobenzene

Examples

Experimental program
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Effect test

Embodiment 1

[0039]A condenser tube and magnetic stirring heating equipment were installed in the 150 ml reaction bottle. Then, 20 grams (0.063 moles) of 1,4-bis(dichloromethyl)tetrafluorobenzene (DCMTFB), 2 grams of 18-crown-6-ether (18-crown-6-ether) and 40 milliliters of acetonitrile ( Acetonitrile) was added in the reaction flask, and the stirring heater was turned on until the temperature of the oil bath was 80° C. and the above-mentioned organic reactants were completely dissolved. Next, 60 grams (0.39 moles) of fluorinating agent CsF were added, and the temperature was raised to 100° C. After reacting for 6 hours, the conversion rate of 1,4-bis(difluoromethyl)tetrafluorobenzene had reached more than 92%. The reaction crude product was treated by filtration, extraction, distillation and sublimation to obtain 12 grams of pure 1,4-bis(difluoromethyl)tetrafluorobenzene with a yield of 76%.

[0040] It is verified by product chemical analysis that the product obtained in this example is...

Embodiment 2

[0050] A condenser tube and magnetic stirring heating equipment were installed in the 150 ml reaction bottle. Then, 30 grams (0.095 moles) of 1,4-bis(dichloromethyl)tetrafluorobenzene (DCMTFB), 45 grams of KF, 45.8 grams of sulfolane (sulpholane) and 3 grams of tetraphenylphosphonium bromide were added to the reaction in the bottle. Turn on the stirring heater, and set the temperature of the oil bath at 125 to 130°C to react for 48 hours. In order to prevent the product from sublimating and overflowing, the outlet of the condenser tube can be plugged with a bottle stopper. Cool to room temperature after the reaction. Then, filter, filter cake with CH 2 Cl 2 After washing, the CH was distilled off under reduced pressure. 2 Cl 2 and 1,4-bis(difluoromethyl)tetrafluorobenzene (DFMTFB). Since 1,4-bis(difluoromethyl)tetrafluorobenzene has sublimation characteristics and accumulates on the condenser, therefore, CH 2 Cl 2 Cleaned, then remove CH 2 Cl 2 6.51 g of 1,4-bis(difl...

Embodiment 3 to 10

[0061] 5.00 grams (0.063 moles) of 1,4-bis(dichloromethyl)tetrafluorobenzene (DCMTFB), 0.50 grams of tetraphenylphosphine bromide (hereinafter referred to as PTC (Br)), 8.50 grams of KF and 30 grams of dimethyl Dimethylformamide (N, N-Dimethylformamide; DMF) was added into the reaction flask. Then, the mixture was heated to 120° C. in an oil bath and stirred with a magnetic stirrer. After 17 hours of reaction, a sample was taken for gas chromatography (GC) analysis, and 4F / 2F / DCMTFB=20.7 / 47.2 / 22.1 (GC area%) was obtained. Among them, 4F (following formula (1)), 3F (following formula (2)), 2F (following formula (3)), 1F (following formula (4)) and DCMTFB (following formula (5)) are respectively as follows ( 1) to (5):

[0062]

[0063] Formula (1) Formula (2)

[0064]

[0065] Formula (3) Formula (4)

[0066]

[0067] Formula (5)

[0068] The preparation method of Examples 4 to 10 is the same as that of Example 3. The relevant reactant dosages, experim...

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Abstract

The invention relates to a method for preparing 1,4-bis(difluoromethyl) tetrafluorobenzene, which comprises the following steps of: (a) mixing 1,4-bis(chloromethyl) tetrafluorobenzene (DCMTFB), a catalyst, an aprotic polar solvent and an alkali metal fluoride to form a reaction solution; (b) heating the reaction solution for reaction; and (c) purifying the reaction solution to obtain the 1,4-bis(difluoromethyl) tetrafluorobenzene.

Description

technical field [0001] The present invention relates to a method for preparing 1,4-bis(difluoromethyl)tetrafluorobenzene (1,4-Bis(difluoromethyl)tetrafluorobenzene), in particular to a method for preparing 1,4-bis(difluoromethyl)tetrafluorobenzene with simple process and high yield. - The method of bis(difluoromethyl)tetrafluorobenzene. Background technique [0002] With the advancement of integrated circuit technology, the design of semiconductor components is gradually developing towards miniaturization and high speed. Due to the need to manufacture more products on a chip with the same area size, the density of components on the chip increases, so two or more layers of metal connections are required for the transmission of components and external signals to provide sufficient area for manufacturing Inner connection wire (Interconnect). Therefore, the transmission speed of external and internal component signals is no longer determined by the switching speed of the gate ...

Claims

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Application Information

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IPC IPC(8): C07C25/13C07C17/14
Inventor 林俊旭涂朝洲何潜渊周娟玉欧伟雄王时俊
Owner YUAN SHIN MATERIALS TECH CORP
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