Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 314084-61-2, name is 2-Bromo-1,3-diethyl-5-methylbenzene, A new synthetic method of this compound is introduced below., Safety of 2-Bromo-1,3-diethyl-5-methylbenzene
Under a nitrogen atmosphere, 14.2 g of malonic acid dinitrile are added at normal pressure and room temperature to a mixture of 67.3 g of 50% potassium hydroxide solution and 300 mi of 1-methyl-2-pyrrolidone. The reaction mixture is heated to from 60 to 100C, and 106 g of diluent are distilled off at reduced pressure (from 20 to 30 mbar). Under a nitrogen atmosphere and at normal pressure, 45.5 g of 2-bromo-1, 3-diethyl-5-methylbenzene are added. The reaction mixture is then heated to 120C with stirring, At that temperature, a mixture of 0.26 g of TRIPHENYLPHOSPHINE, 0.2 g of a commercially available palladium (LI) chloride solution in concentrated hydrochloric acid (20% Pd content corresponding to 0.071 g of palladium (II) chloride and 0.142 g of concentrated hydrochloric acid) and 19.5 g of 1-METHYL-2-PYRROLIDONE is added. Stirring is carried out at from 120 to 125C FOR 1 hour, and then a mixture of 0.26 g of triphenylphosphine, 0.2 g of a commercially available PALLADIUM (II) chloride solution in concentrated hydrochloric acid (20% Pd content corres- ponding to 0.071 g of palladium (li) chloride and 0.142 g of concentrated hydrochloric acid) and 19.5 g of 1-METHYL-2-PYRROLIDONE is again added. The reaction mixture is stirred for 3 hours at from 120 to 125C, and then a further 237 g of diluent are distilled off at reduced pressure (from 20 to 30 mbar) and at from 80 to 120C. After cooling the reaction mixture to 45C, 100 mi of toluene and 220 g of water are added and intensive stirring is carried out for 15 minutes. The two-phase mixture is transferred to a separating funnel in order to be separated. The organic phase is discarded. The aqueous phase is isolated and and 43.4 g of material are distilled off at reduced pressure (from 250 to 300 mbar) and at from 70 to 110C. 48.5 g of 32% hydrochloric acid are added in the course of from 60 to 80 minutes to the distillation sump, during the course of which the product crystallises out and the pH value falls to from 4.0 to 4.5. Suction filtration is carried out followed by washing with 130 ml of water (divided into 2 portions). The product is dried in a vacuum drying cabinet for 16 hours at from 100 to 250 mbar. 37.2 g (content 97.7% ; yield 85.7%) of 2- (2, 6-diethyl-4- methylphenyl) malonic acid dinitrile are obtained.
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Patent; SYNGENTA PARTICIPATIONS AG; WO2004/50607; (2004); A1;,
Bromide – Wikipedia,
bromide – Wiktionary