P-Dimethylaminobenzaldehyde is an organic intermediate, which can be prepared from n, N-dimethylaniline and DMF. It is reported in the literature that p-Dimethylaminobenzaldehyde can be used to prepare high-purity DAST source powder, and can also be used to make color developing solution to analyze aminohydroxyurea.
Add 4.9g (0.032mol) of phosphorus oxychloride into a 100ml three necked bottle, slowly add 2.5G (0.031mol) of DMF under an ice bath, drop it for 8min, stir it for 10min, slowly add 3.66g (0.03mol) of N, N-dimethylaniline into a three necked bottle for 10min, drop it, and transfer the reaction solution to a boiling water bath for reaction for 2h. After the reaction, pour the reaction solution into 20ml of ice water, adjust pH = 4 with 30% sodium hydroxide solution, let it stand for crystallization, and filter it by suction the next day, A light yellow or nearly colorless solid was obtained and recrystallized with 30ml of ethanol water (1:2.5v/v) to obtain the product p-Dimethylaminobenzaldehyde.
Application i
Cn201410570172.2 discloses a synthesis process of DAST source powder with high yield and purity. The synthesis process is divided into two steps:
1. 4-methyl-n-methylpyridine p-toluenesulfonate in absolute ethanol was prepared by reacting 4-methylpyridine with methyl p-toluenesulfonate in absolute ethanol;
2. DAST source powder with high yield of 85-95% and high purity of 90-95% can be obtained by the reaction of 4-methyl-n-methylpyridine p-toluenesulfonate with p-Dimethylaminobenzaldehyde in absolute ethanol as solvent and under the catalysis of n-butylamine or piperidine. Absolute ethanol is used as the reaction solvent, which avoids the harm of toxic and harmful solvents such as toluene and methanol to the operator's body, and reduces the pollution of waste liquid to the environment;
The success of the research and development of the invention is conducive to the cultivation of high-quality and large-size DAST crystals, which lays a good material and theoretical foundation for the research of DAST crystals and related products.
Application II
Cn201210035819.2 discloses an analytical method for hydroxysemicarbazide in plutonium solution after uranium plutonium separation, which comprises the following steps:
(1) Dissolve p-Dimethylaminobenzaldehyde in ethanol solvent to prepare a color developing solution;
(2) Dilute the plutonium solution containing uranium and plutonium with nitric acid 10-1000 times (pH value is - 0.2-1), and add the solution to be tested diluted with nitric acid to the color developing solution;
(3) Allowing the color developing system of step (2) to undergo a color reaction at a temperature of 15 to 30 ℃ for at least 5 minutes;
(4) With the blank solution as the reference, the absorbance value a of the color developing system was measured at the wavelength of 430 ~ 490nm;
(5) According to the measured absorbance value a, combined with the concentration absorbance value curve of hydroxysemicarbazide in the color development system, the solution can be obtained. The method of the invention is simple and convenient, and does not require special instruments; The measured values obtained by this method are in good agreement with the theoretical values.
Application III
Cn201710234643.6 discloses a method for analyzing the content of hydroxysemicarbazide in the post-treatment process of nuclear fuel Purex. The analysis method comprises the following steps:
(1) Mix the test solution containing aminohydroxyurea in the nuclear fuel Purex post-treatment process with p-Dimethylaminobenzaldehyde and acid solution, and heat it for color reaction;
(2) The solution after color development is cooled to room temperature, and the absorbance is measured at the wavelength of 456nm. The content of hydroxysemicarbazide in the test solution containing hydroxysemicarbazide is determined according to the standard working curve. By using the method for analyzing the content of hydroxysemicarbazide in the nuclear fuel Purex post-treatment process of the present invention, the content of hydroxysemicarbazide in the nuclear fuel Purex post-treatment process can be analyzed with good precision, selectivity, accuracy, stability and simple operation.
Application IV
Cn200710061286.4 discloses a preparation method of a surface complexing indicator rose red silver reagent. The preparation steps are as follows:
(1) Put rhodanine, p-Dimethylaminobenzaldehyde and glacial acetic acid in a flask with a condenser, put the flask in an electric heating jacket, raise the temperature to reflux, and reflux for 2-4 hours;
(2) The reaction product was poured out and filtered;
(3) The filtered filter cake is recrystallized with ethanol and dried at 50-70 degrees Celsius to obtain a finished product, which is rose red needle shaped crystal.
The preparation method of the invention is simple, easy to realize, short in production time and high in production efficiency. The rose red silver reagent prepared by the method of the invention has high sensitivity, strong stability, good detection effect, simple and easy use method, reduced operation difficulty and improved work efficiency.