Continuously updated synthesis method about 1939-27-1

At the same time, in my other blogs, there are other synthetic methods of this type of compound, N-(3-(Trifluoromethyl)phenyl)isobutyramide, and friends who are interested can also refer to it.

Synthetic Route of 1939-27-1, 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. 1939-27-1 name is N-(3-(Trifluoromethyl)phenyl)isobutyramide, 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.

Step 3, put a 100ml three-necked bottle with mechanical stirring and thermometer into the ice machine, add 23ml of concentrated sulfuric acid, stir,Addition of 10.75g of iso – butyramide benzotrifluoride until the solid dissolves, keeping the temperature at -5 C, adding 2.3ml of 95% fuming HN03, stirring 3h; Step 4, the above reaction was poured into a certain amount of ice water mixture, was sticky solid, add 80g toluene, stirring,Separation, the upper organic phase was washed three times with 3% sodium bicarbonate solution, followed by three washes, and the solvent was removed by rotary evaporation to give a yellow solid; Step 5, the above yellow solid was added to the flask, 20 ml of ethanol was added, and the mixture was heated to reflux, solid 1% of activated carbon was added, stirred for 5 minutes, and hot filtered.The filtrate was cooled to room temperature, and petroleum ether was slowly added thereto until the solution became turbid. The solution was refrigerated at 0C for 3 hours, filtered, and dried at 60C to obtain flunitamide as a pale yellow solid.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, N-(3-(Trifluoromethyl)phenyl)isobutyramide, and friends who are interested can also refer to it.

Reference:
Patent; Xuzhou Nuokefei Pharmaceutical Technology Co., Ltd.; Zhao Qingling; Li Weixin; (7 pag.)CN108003051; (2018); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics