Preparation process of 3-amino-4-cetyl chlorobenzoate
A technology of chlorobenzoic acid and cetyl ester, which is applied to the preparation of organic compounds, chemical instruments and methods, and the preparation of cyanide reactions. It can solve the problems of difficult reactions, difficult separations, and high production costs. Treatment process, increase reaction speed, good catalytic effect
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[0027] The invention provides a preparation method of hexadecyl 3-amino-4-chlorobenzoate, which uses 3-amino-4-chlorobenzoic acid and cetyl alcohol as the main reaction raw materials, and selects tin tetrachloride or stannous chloride Or use tetrabutyl titanate as a catalyst, dehydrate through solvent reflux, and prepare hexadecyl 3-amino-4-chlorobenzoate through esterification. Common toluene, xylene and chlorobenzene are used as reaction solvents, and the reaction is carried out under reflux, the reaction process is easy to control, and the end point is easy to determine.
[0028] Examples are listed below to specifically illustrate the technical solution of the present invention. But these are just application examples, they are given as examples only, and should not be regarded as limitations on the application of the present invention. All equivalent replacements or equivalent transformations of operating conditions fall within the protection scope of the present inventi...
Embodiment 1
[0030] A 1000ml four-necked round-bottomed flask with mechanical stirring, thermometer, water separator, condenser tube, in the flask was added successively 200g of toluene, 200g of 3-amino-4-chlorobenzoic acid and 335g of cetyl alcohol. After heating up and dissolving, add 5g of tin tetrachloride under stirring. Heat up and reflux for dehydration, and the reaction is considered to be over when no more water comes out. The solvent was recovered under reduced pressure, and the obtained toluene could be used repeatedly. The residue was added into 1400ml of methanol under stirring, cooled to 25°C and filtered to obtain a crude product. The crude product was refined with 1400ml of methanol, and dried to obtain 330g of hexadecyl 3-amino-4-chlorobenzoate, with a yield of 72%. High-performance liquid chromatography analysis shows that the content of hexadecyl 3-amino-4-chlorobenzoate is 99.5% in the product, and gas chromatography analysis shows that the content of hexadecyl 3-amino...
Embodiment 2
[0032] A 2000ml four-necked round-bottomed flask with mechanical stirring, thermometer, water separator, and condenser tube, added 500g xylene, 200g of 3-amino-4-chlorobenzoic acid and 335g of cetyl alcohol successively in the flask. After heating up and dissolving, add 40g of tin tetrachloride under stirring. Heat up and reflux for dehydration, and the reaction is considered to be over when no more water comes out. The solvent was recovered under reduced pressure, and the obtained xylene could be used repeatedly. The residue was added into 1400ml of methanol under stirring, cooled to 25°C and filtered to obtain a crude product. The crude product was refined with 1400ml of methanol, and dried to obtain 300g of hexadecyl 3-amino-4-chlorobenzoate, with a yield of 65%. High performance liquid chromatography analysis shows that the content of hexadecyl 3-amino-4-chlorobenzoate is 99.4% in the product, and gas chromatography analysis shows that the content of hexadecyl 3-amino-4-c...
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