Electric Literature of 39538-68-6, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 39538-68-6 as follows.
5.2 g of 2-methoxy-4-methylaniline was dissolved in 32 ml of water and 11.4 ml of concentrated hydrochloricacid, cooled to 0-5 C in an ice bath, and 2.88 g of sodium nitrite dissolved in 9 ml of water was added dropwise to theabove cooled solution. The mixture was stirred for 10 minutes in an ice bath and then 5.6 g of sodium acetate was added.The above reaction liquid was added dropwise to a hot (about 75 C) solution wherein 11 g of potassium ethyl xanthatewas dissolved in 51 ml of water, stirred for another 1 hour, cooled to room temperature, and extracted with ethyl acetate.After liquid separation, the organic phase was washed with saturated aqueous solution of sodium chloride and thendried over anhydrous sodium sulfate, filtered, concentrated, and then dissolved in a solution of 1.3 N potassium hydroxidein ethanol, and then added with 3 g of glucose and refluxed for 3 hours. The reaction mixture was concentrated and thepH was adjusted to about 1 with 6 N sulfuric acid in ice bath, and then 5.7 g of zinc powder was added and heated andstirred at 50 C for 30 minutes. The insoluble was filtered off and the filtrate was extracted with ethyl acetate. After liquidseparation, the organic phase was washed with saturated aqueous solution of sodium chloride and dried over anhydroussodium sulfate, filtered and concentrated, and the residue was separated by column chromatography (100% petroleumether) to afford 4.15 g of oily matter, yield 71%.1H NMR (300 MHz, DMSO-d6) delta 7.17 (s, 1H), 6.81 (s, 1H), 6.66 (s, 1H), 4.63 (s, 1H), 3.80 (s, 3H), 2.26 (s, 3H).
According to the analysis of related databases, 39538-68-6, the application of this compound in the production field has become more and more popular.