Synthetic Route of 30448-43-2, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 30448-43-2 name is Di-tert-butyl phthalate, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.
General procedure: To a 500 ml four-necked flask equipped with a stirring, a thermometer, a distillation apparatus, and a constant pressure dropping funnel, 200 g of toluene and 17.0 g of potassium t-butoxide (0.15 mol) were added, and the mixture was heated to an internal temperature of 100-105 C. 27.8 g (0.1 mol) of di-tert-butyl phthalate and 20.0 g (0.12 mol) of a mixture of tert-butyl 3-cyanobutanoate were added dropwise, while t-butanol was distilled off, and the mixture was stirred at 100 C for 3 hours. . Cool to 20-25 C, add 20 grams of 20% aqueous sodium hydroxide solution, stir the reaction at 20-30 C for 3 hours; connect the tail gas absorption device with lye, then add 30% hydrochloric acid to the reaction bottle to adjust the pH value The reaction was stirred at 2.0-2.5, 60 C for 3 hours; the layers were separated, and the aqueous layer was extracted with toluene three times, 50 g each time. The organic phases were combined, and toluene was distilled away to give 15.8 g of 2-methyl-1,4-naphthoquinone in a yield of 91.9%. The purity of GC was 99.7%.
At the same time, in my other blogs, there are other synthetic methods of this type of compound, Di-tert-butyl phthalate, and friends who are interested can also refer to it.
Reference:
Patent; Xin Fa Pharmaceutical Co., Ltd.; Qi Yuxin; Qu Hu; Ju Lizhu; (6 pag.)CN109384659; (2019); A;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics