Fluorine-containing coupling agent and preparation method and application thereof
A coupling agent and fluorine-containing alcohol technology, applied in the field of fluorine-containing coupling agents and their preparation, can solve the problems of difficult preparation of amide compounds, harsh reaction conditions, environmental pollution, etc., and achieve a wide range of substrates and efficient synthesis. , Environmentally friendly effect
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0040] The synthesis of 2-chloro-4,6-bis(octafluoropentyloxy)-1,3,5-triazine, the synthetic route is shown in the figure below:
[0041]
[0042] Specifically include the following steps:
[0043] (1) Tripolychlorazine (3.68g, 0.02mol) and 40mL of anhydrous dichloromethane were added to a 250mL three-necked flask, and 2 Protect and stir evenly at 0-5°C, then add sodium hydroxide (3.2g, 0.08mol) into the reaction flask and continue stirring.
[0044] (2) Dilute octafluoropentanol (7mL, 0.05mol) with dichloromethane (20mL) and slowly add it dropwise into a three-neck flask, react at 0-5°C for 2h, then slowly raise the temperature to reflux, react for 4h, stop reaction.
[0045] (3) Wash the reaction solution repeatedly with deionized water, 5% HCl solution and deionized water in sequence until neutral. Rotary evaporation to remove CH 2 Cl 2and excess octafluoropentanol to obtain fluorine-containing coupling agent 2-chloro-4,6-bis(octafluoropentyloxy)-1,3,5-triazine. The...
Embodiment 2
[0048] The synthesis of 2-chloro-4,6-bis(tetrafluoropropoxy)-1,3,5-triazine, the synthetic route is shown in the figure below:
[0049]
[0050] Specifically include the following steps:
[0051] (1) Tripolychlorazine (3.68g, 0.02mol) and 40mL of anhydrous dichloromethane were added to a 250mL three-necked flask, and 2 Protect and stir evenly at 0-5°C, then add sodium hydroxide (3.2g, 0.08mol) into the reaction flask and continue stirring.
[0052] (2) Dilute tetrafluoropropanol (4.44mL, 0.05mol) with dichloromethane (20mL) and slowly drop it into a three-neck flask, react at 0-5°C for 2h, then slowly raise the temperature to reflux, and react for 4h, Stop responding.
[0053] (3) Wash the reaction solution repeatedly with deionized water, 5% HCl solution and deionized water in sequence until neutral. Rotary evaporation removes CH2Cl2 and excess tetrafluoropropanol to obtain fluorine-containing coupling agent 2-chloro-4,6-bis(tetrafluoropropoxy)-1,3,5-triazine. The char...
Embodiment 3
[0056] The synthesis of benzoic acid benzamide, the synthetic route is as shown in the figure below:
[0057]
[0058] Specifically include the following steps:
[0059] (1) The fluorine-containing coupling agent 2-chloro-4,6-bis(octafluoropentyloxy)-1,3,5-triazine (2g, 3.48mmol) prepared in Example 1 and N-methyl Morpholine (0.35g, 3.48mmol) joins in the reactor, adds 40mL anhydrous tetrahydrofuran, under N 2 Protection, stirring at 0-5°C for 15 minutes;
[0060] (2) Add benzoic acid (0.424g, 3.48mmol) to the reaction solution, continue to react for 30min, then add aniline (0.324g, 3.48mmol) to the reactor, react at room temperature for 12h, and stop the reaction;
[0061] (3) filtering to remove solid impurities, rotary evaporation to remove the organic solvent, and recrystallization with ethanol to obtain benzoic acid benzamide.
[0062] image 3 H NMR spectrum of benzamide benzoate. From image 3 It can be seen that the peak at 7.81ppm is the hydrogen on the amide...
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More