Continuously updated synthesis method about 39538-68-6

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-Methoxy-4-methylaniline, and friends who are interested can also refer to it.

Related Products of 39538-68-6, 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. 39538-68-6 name is 2-Methoxy-4-methylaniline, 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.

A solution of sodium nitrite (7 g, 101.4 mmol) in water (25 ml) was added dropwise to a cooled (0-5C) solution of Intermediate 1A (13.7 g, 100 mmol) in concentrated hydrochloric acid (30 ml) and water (85 ml). After stirring at 0C for 10 min, sodium acetate (15 g, 182.8 mmol) was added. The resulting mixture was added dropwise to a hot solution (70-80C) of potassium O-ethyl dithio- carbonate (30 g, 187.1 mmol) in water (140 ml), stirred between 70C and 80C for 1 h and then cooled to rt. The mixture was extracted twice with ethyl acetate, and the combined organic extracts were dried over sodium sulfate and evaporated. The residue was taken up in a 1.3 M solution of potassium hydroxide in ethanol (300 ml). Glucose (8 g) was added, and the resulting mixture was refluxed for 3 h. Then, the ethanol solvent was evaporated, and the residue was diluted with water and acidified with 6 N aqueous sulfuric acid. Zinc powder (15 g) was added carefully, and the resulting mixture was heated to 50C for 30 min. The mixture was then cooled to rt, diluted with dichloromethane and filtered. The filtrate was extracted twice with dichloromethane, and the combined organic extracts were dried over sodium sulfate and evaporated affording 14.3 g of the crude product which was used in the next step without further purification.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-Methoxy-4-methylaniline, and friends who are interested can also refer to it.

Reference:
Patent; BAYER INTELLECTUAL PROPERTY GMBH; BAYER PHARMA AKTIENGESELLSCHAFT; COLLIN, Marie-Pierre; BROHM, Dirk; HEROULT, Melanie; LOBELL, Mario; HUeBSCH, Walter; LUSTIG, Klemens; GRUeNEWALD, Sylvia; BOeMER, Ulf; VOeHRINGER, Verena; LINDNER, Niels; WO2013/87647; (2013); A1;,
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