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ChemicalBook CAS DataBase List Diflufenican

Diflufenican synthesis

3synthesis methods
-

Yield:83164-33-4 88%

Reaction Conditions:

with dmap;1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride in dichloromethane at 20;Cooling with ice;

Steps:

4 Example 4: Synthesis of fluoxachlor
In a 50 mL round bottom flask, add 2,4-difluoroaniline (65.0 mg, 0.5 mmol), 2-(3-trifluoromethyl)phenoxynicotinic acid E1 (170.0 mg, 0.6 mmol), 10 mL of anhydrous dichloromethane (DCM) was added, and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (EDCI · HCl, 124.5 mg, 0.65 mmol) was added under an ice bath. 4-Dimethylaminopyridine (DMAP, 1.2mg, 0.01mmol), the mixed system was stirred at room temperature, after TLC detected the reaction was complete, Saturated sodium bicarbonate (NaHCO3, 5 mL) was added to quench the reaction, and extracted with dichloromethane (DCM) three times (10 mL × 3), Washed with water (10mL × 3), washed with saturated sodium chloride solution (10mL × 3), dried over anhydrous sodium sulfate (Na2SO4), concentrated under reduced pressure, and separated by column chromatography (V petroleum ether: V ethyl acetate, 8:1) ,173mg of Diflufenican was obtained as a white solid with a yield of 88%.

References:

Nanjing Agricultural University;Li Shengkun;Song Zehua;Wang Guotong;Li Wei CN110872283, 2020, A Location in patent:Paragraph 0048-0052

FullText

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