* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Reference：
[1] Bulletin de la Societe Chimique de France, 1905, vol. <3> 33, p. 273[2] Annales de Chimie (Cachan, France), 1905, vol. <8> 6, p. 240
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Reference：
[1] Bulletin de la Societe Chimique de France, 1905, vol. <3> 33, p. 273[2] Annales de Chimie (Cachan, France), 1905, vol. <8> 6, p. 240
General procedure: In the continuous reaction apparatus, a mixture of o-xylene, dimethyl phthalate, manganese acetate, cobalt acetate and potassium acetate was poured into an oxidation reaction tube (the reaction mixture had a cobalt, manganese and potassium ion concentration of 300 ppm each, O-xylene concentration of 30%), filled with 3MPa oxygen, 200 C under the oxidation, reaction residence time of 2h. The mixture of the oxidized mixture and the methanol was poured into an esterification reaction tube (molecular weight ratio of methanol to starting o-xylene) of 10: 1, The mass ratio of molecular weight of aluminum silicate phosphate to starting o-xylene was 1: 100), and the reaction time was 3h at 150 c. After the esterification reaction, the mixture is oxidized to the second methyl group on the benzene ring, and then the esterification reaction is carried out in the esterification reaction tube. After the reaction, the mixture was subjected to gas chromatography and liquid chromatography to calculate the one-way conversion of o-xylene and the selectivity of dimethyl phthalate. The specific practice of Examples 2 to 18 is similar to that of Example 1, and the specific reaction conditions and results are shown in Table 1.
With water; potassium hydroxide; In dimethyl sulfoxide; at 0℃; for 3.5h;
General procedure: A diester (1.2mmol) was dissolved in the specified amount of THF or DMSO, and the specified amount of water was added. The reaction mixture was immersed in an ice-water bath and cooled to 0C. To this reaction mixture, 4mL of 0.5M KOH was added in small portions with stirring until the starting diester was consumed accordingto TLC. The reaction was stirred at the same temperature. It was then acidified with 1.0M HCl at 0C, saturated with NaCl, extracted with ethyl acetate three to four times, and dried over Na2SO4. The extracts were evaporated in vacuo and purified by silica gel column chromatography to afford the desirable half-ester.
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