Unlock instant, AI-driven research and patent intelligence for your innovation.

A method for rapidly preparing 2,2-bis(4-(4-aminophenoxy)phenyl)hexafluoropropane and its intermediates at low temperature

A technology of aminophenoxy and hexafluoropropane, which is applied in the field of compounds, can solve problems such as unsuitability for industrial production and waste water generation, and achieve the effects of reducing production costs and increasing product yields

Inactive Publication Date: 2017-09-22
GUANGXI UNIVERSITY OF TECHNOLOGY
View PDF8 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Moreover, there will still be a large amount of waste water, which is not suitable for industrial production.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A method for rapidly preparing 2,2-bis(4-(4-aminophenoxy)phenyl)hexafluoropropane and its intermediates at low temperature
  • A method for rapidly preparing 2,2-bis(4-(4-aminophenoxy)phenyl)hexafluoropropane and its intermediates at low temperature
  • A method for rapidly preparing 2,2-bis(4-(4-aminophenoxy)phenyl)hexafluoropropane and its intermediates at low temperature

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Prepare a 1000ml three-neck flask, equipped with a mechanical stirring and distillation device, add 33.6g (0.1mol) of 2,2-bis(4-hydroxyphenyl)hexafluoropropane, 400g of water, C-10.007g (0.00001mol) of potassium carbonate 27.6 g (0.2mol), 34.66g (0.22mol) of p-chloronitrobenzene, under nitrogen protection, the temperature was raised to 70°C, reacted for 8 hours, cooled to 1°C, filtered, dried, and the obtained solid was washed with 800 milliliters of ethanol and 200 54.9 g of 2,2-bis(4-(4-nitrophenoxy)phenyl)hexafluoropropane was obtained by recrystallization from a mixed solvent of ethyl acetate in milliliter. HPLC 99.6%, mp 159.7°C; yield 95%.

[0049] Add 54.9 g of 2,2-bis(4-(4-nitrophenoxy)phenyl)hexafluoropropane, 600 ml of ethyl acetate, and 8 g of 5% palladium carbon into the stainless steel hydrogenation kettle. 30°C, controlled 0.05MPa hydrogen reduction reaction for 6 hours, the reaction is complete. Stop reaction, after nitrogen replacement, take out materi...

Embodiment 2 to Embodiment 33

[0054] In Example 2-Example 33, the difference is in the process of preparing 2,2-bis(4-(4-nitrophenoxy)phenyl)hexafluoropropane, the type of halogenated nitrobenzene, the solvent The type and proportion of the catalyst, the type and amount of the catalyst, the type of alkali, one or more of the different reaction temperatures, all the other specific parameters and amounts and the preparation method are the same as in Example 1, and the specific conditions are as shown in Table 2A and Table 2B Shown:

Embodiment 2- Embodiment 20

[0056]

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention provides a method for low temperature rapid preparation of a 2, 2-bis(4-(4-aminophenoxy)phenyl)hexafluoropropane intermediate. The 2, 2-bis(4-(4-aminophenoxy)phenyl)hexafluoropropane intermediate is 2, 2-bis(4-(4-nitrophenoxy)phenyl)hexafluoropropane, and is obtained by reacting 2, 2-bis(4-(4-hydroxyphenyl)hexafluoropropane with para-halogenated nitrobenzene in the presence of a solvent, a catalyst A and alkali. The invention also provides the method for low temperature rapid preparation of 2, 2-bis(4-(4-aminophenoxy)phenyl)hexafluoropropane. The method provided by the invention adopts low temperature operation, and can complete the intermediate preparation after 8h of reaction at 65-80DEG C. The method can improve the product yield to over 78%, and also can reduce the production cost.

Description

technical field [0001] The invention belongs to the technical field of compounds, in particular to a method for rapidly preparing 2,2-bis(4-(4-aminophenoxy)phenyl)hexafluoropropane and its intermediate at low temperature. Background technique [0002] 2,2-bis(4-(4-aminophenoxy)phenyl)hexafluoropropane (4-BDAF for short), English name 2,2-bis(4-(4-aminophenoxy(-phenyl)-hexa- Fluoropropane, molecular formula: C27H20F6N2O2, structural formula as shown in formula (I): [0003] [0004] 4-BDAF is one of the main raw materials for the preparation of liquid crystal alignment materials for thin film transistor liquid crystal displays (TFT-LCD), and is widely used in the preparation of fluorine-containing vulcanization accelerators and thermoplastic resins. It is involved in WO02100949, WO2004011528, and US5504128 . [0005] The preparation method of existing 4-BDAF mainly contains following several kinds: [0006] Method 1: The reaction formula is as follows [0007] [00...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07C205/38C07C201/12C07C217/90C07C213/02
Inventor 蒋旭东王占奇
Owner GUANGXI UNIVERSITY OF TECHNOLOGY