The preparation method of benzophenone acid compound
A technology of benzophenone acid and compound, which is applied in the field of preparation of pressure-sensitive dye intermediates, can solve the problems of increasing the preparation cost of benzophenone acid compound, increasing environmental pollution, reducing operation safety and the like, and achieves convenient industrial production, Reduce the effect of easy control of operation process and reaction conditions
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0031] 1) Add 20.7g (0.1mol) N-ethyl-N-isoamyl m-aminophenol and 20.7g (0.14mol) phthalic anhydride to a 100mL single-necked bottle, stir, slowly heat to 80°C, and keep the reaction 9h, react at 90°C for 10h, thin layer chromatography (TLC) showed that the reaction of the raw materials was basically complete, the reaction was stopped, and the reaction mixture was obtained;
[0032] 2) Add 30 mL of water and 20 mL of toluene into the reaction mixture obtained in step 1), keep stirring at 80°C for 30 minutes, and after standing, separate liquids while hot;
[0033] 3) the lower water phase is cooled and crystallized, filtered to obtain the crude product of phthalic acid, and the crude product of phthalic acid is purified to obtain the phthalic acid of white needle-like crystals by conventional methods, HPLC: greater than 99%, recovery The rate is 22% (calculated with the total amount of phthalic anhydride used); the upper organic phase is transferred into a 100mL three-necked fl...
Embodiment 2
[0036] 1) Add 16.5g (0.1mol) N,N-diethyl-m-aminophenol, 17.8g (0.12mol) phthalic anhydride to a 100mL single-necked bottle, stir, slowly heat to 110°C for 9h, TLC Method (TLC) showed that the basic reaction of the raw materials was basically complete, and the reaction was stopped to obtain a reaction mixture;
[0037] 2) Add 30 mL of water and 20 mL of toluene into the reaction mixture of step 1), keep stirring at 80°C for 60 minutes, and thermally separate the liquid;
[0038] 3) The lower water phase is cooled and crystallized, and the crude product of phthalic acid is filtered to obtain the crude product of phthalic acid. The crude product of phthalic acid is purified by conventional methods to obtain the phthalic acid of white needle crystals, HPLC: more than 99%, recovery rate 10% (calculated with the total amount of phthalic anhydride used); the upper organic phase is transferred into a 100mL there-necked flask, and 30mL of sodium hydroxide solution with a mass concentra...
Embodiment 3
[0041] 1) Add 22.1g (0.1mol) N,N-dibutyl-m-aminophenol and 17.8g (0.12mol) phthalic anhydride into a 100mL single-necked bottle, stir, slowly heat to 90°C for 6 hours, and then react at 100°C 8h, thin layer chromatography (TLC) showed that the reaction of the raw materials was basically complete, and the reaction was stopped to obtain a reaction mixture;
[0042] 2) Add 30 mL of water and 20 mL of xylene to the reaction solution, keep stirring at 80°C for 50 minutes, and thermally separate the solution;
[0043] 3) lower water phase, cooling and crystallization, filtered to obtain the crude product of phthalic acid, purified to obtain the phthalic anhydride of white needle-like crystals, HPLC: greater than 99%, recovery rate 12% (with the phthalic anhydride used) The upper organic phase was transferred into a 100mL three-necked flask, and 20mL of sodium hydroxide solution with a mass concentration of 40% was added dropwise with heating and stirring, and a large amount of solid...
PUM
| Property | Measurement | Unit |
|---|---|---|
| recovery rate | aaaaa | aaaaa |
Abstract
Description
Claims
Application Information
Login to View More