PropanaMide, 2-Methyl-N-[4-(trifluoroMethyl)phenyl]- synthesis

Yield:1978-70-7 40%

Reaction Conditions:

with copper diacetate in water;1,2-dichloro-ethane at 80; for 20 h;Schlenk technique;Sealed tube;

Steps:

20

Take a 25 mL Schlenk tube equipped with a magnetic stir bar, and fill it with asymmetric diaryliodonium salt (0.3 mmol) and Cu(OAc) 2 (5.5 mg, 0.03 mmol). DCE (2.0 mL), H 2 O (0.9 mmol) and isobutyronitrile (0.9 mmol) were sequentially added from a syringe, and the tube was sealed at 80° C. and stirred for 20 hours. The resulting solution was then cooled to room temperature and extracted with EtOAc (3×15 mL). The combined organic layer was washed with brine, and dried over anhydrous Na2SO4. The volatiles were removed in vacuo, and the residue was purified by column chromatography to obtain a pure product with a yield of 40%. Its structural formula was as follows, and then the structure was identified by melting point, nuclear magnetic and mass spectrometry.

References:

CN111302967,2020,A Location in patent:Paragraph 0123-0127