Introduction of a new synthetic route about 31599-60-7

Statistics shows that 31599-60-7 is playing an increasingly important role. we look forward to future research findings about 1-Iodo-2,3-dimethylbenzene.

31599-60-7, name is 1-Iodo-2,3-dimethylbenzene, belongs to iodides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. 31599-60-7

Under nitrogen protection, 24 g of magnesium turnings (1 mol) and 160 ml of tetrahydrofuran were added to a reaction flask and stirred at room temperature18.5 g was added dropwise2,3-dimethyliodobenzene (0.1 mol) and100 ml of tetrahydrofuran,Triggering reaction,Then, 166.5 g of 2,3-dimethyliodobenzene (0.9 mol) was added dropwise1000 ml of tetrahydrofuran mixture, drop finished, reflux reaction 1hour. The resulting Grignard reagent was cooled in an ice bath, and 73 g of N, N-dimethylformamide (1.0 mol) and 300 ml of tetrahydrofuranFuran mixture to control the reaction temperature is not higher than 30 degrees, dropping is completed at room temperature for 5 hours. After completion of the reaction1000 ml of saturated ammonium chloride solution for 1 hour hydrolysis, and then separated from the organic phase, the aqueous phase extracted with ethyl acetate aThe organic phase was washed with 500 mL of saturated brine and allowed to stand for separation. The organic phase was stirred and dried with 50 g of anhydrous sodium sulfate1 hour, filtered and the filtrate was concentrated to dryness under reduced pressure to give 2,3-dimethylbenzaldehyde in a yield of 93% and a purity of 95%

Statistics shows that 31599-60-7 is playing an increasingly important role. we look forward to future research findings about 1-Iodo-2,3-dimethylbenzene.

Reference:
Patent; Suo Anke (Shanghai) Investment Co; Mao, Zhenjun; Jiang, Xindong; Lin, Xufeng; Li, Qingpo; You, Jian; (5 pag.)CN105503551; (2016); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com