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ChemicalBook CAS DataBase List 5-Methoxy-1-[4-(trifluoromethyl)phenyl]-1-pentanone

5-Methoxy-1-[4-(trifluoromethyl)phenyl]-1-pentanone synthesis

6synthesis methods
-

Yield:61718-80-7 90.5%

Reaction Conditions:

Stage #1: 4-(methoxy)-1-chlorobutanewith magnesium;methyl iodide in tetrahydrofuran at 75; for 13 h;Inert atmosphere;
Stage #2: methyl 4-(trifluoromethyl)benzoate in tetrahydrofuran at 20 - 70;Inert atmosphere;

Steps:

2.2 The synthesis method of 1-p-trifluorotolyl-5-methoxy-pentanone, the specific synthesis process is as follows:

(2) Under the protection of nitrogen, add 1500 mL of anhydrous tetrahydrofuran and 108 g of magnesium turnings to the flask, and add a few drops of methyl iodide to raise the temperature to 75 ° C.After stirring and dissolving, 602.1 g of 1-chloro-4-methoxybutane was added dropwise. After the completion of the dropwise addition, the reaction was kept at a constant temperature for 13 hours. After cooling to room temperature, 45.88 g of methyl p-trifluoromethylbenzoate prepared in the step 1 was added dropwise. ,5 g was added dropwise per minute, and the mixture was heated to 70 ° C for 4-6 hours. After being completely cooled, glacial hydrochloric acid was poured into the reaction solution.The solvent tetrahydrofuran is separated by extraction, and the extracted tetrahydrofuran is concentrated. The aqueous layer obtained after extraction is extracted with dichloromethane, and the oil phase is added to the concentrate of tetrahydrofuran.The extract product was obtained, and the obtained product was dried and dried over anhydrous sodium sulfate, and evaporated to give 152.36 g of the product 1- p-trifluorotolyl-5-methoxy-pentanone.The yield of the product was 90.5%, and the reaction structural formula is shown in Fig. 1.

References:

CN108191630,2018,A Location in patent:Paragraph 0024; 0025; 0027

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