Electric Literature of 120-61-6, A common heterocyclic compound, 120-61-6, name is Dimethyl terephthalate, molecular formula is C10H10O4, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
This example demonstrates the preparation of 4-chlorocarbonyl- benzoic acid methyl ester having the following structure. In a 4 L kettle with mechanical stirrer, reflux condenser, addition funnel, thermometer, water bath and hot plate, 438 g dimethyl terephthalate (DMT) and 2700 mL toluene were added. The kettle was heated to about 65 00 to dissolve all the DMT. After dissolution, a potassium hydroxide solution (144.54 g in 700 mL methanol) was added dropwise over 45 minutes. The reaction was stirred at 65 00 for three hours and then the reaction cooled to room temperature overnight. The solid was collected after filtration and washed with 3750 mL toluene at 80 00. The product was filtered again and dried in the oven at 110 00. The yield was 465.9 g(95.3%).In a 2 Lthree neck round bottom flask with mechanical stirrer, addition funnel, water bath, thermometer, nitrogen sweep, and hot plate, 130.31 g of the product made in previous step and 1000 mL toluene were added. Then 48 mL of thionyl chloride was added dropwise. After the completion of addition, the mixture was heated to 67 00 for three hours. The reaction cooled to room temperature and was stirred overnight. The contents were filtered to collect the filtrate. The excess solvent was removed by vacuum and 86.52 g of product was obtained (73% yield).
The synthetic route of 120-61-6 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; MILLIKEN & COMPANY; MILEY, John W.; QIN, Haihu; DOTSON, Darin L.; COOLEY, Mary Angela; TSAI, Chi-Chun; DEY, Sanjeev K.; TORRES, Eduardo; ALVAREZ, Francisco; WO2015/42561; (2015); A1;; ; Patent; MILLIKEN & COMPANY; QIN, Haihu; DOTSON, Darin L.; TORRES, Eduardo; DEY, Sanjeev K.; ALVAREZ, Francisco; WO2015/42563; (2015); A1;,
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