Sodium hydride → HCID 86719001, compound

Participants

Reaction Steps

NaH (4.39 g) was suspended in THF/DMSO (400 mL) and Me3S—I (35.4 g) was added carefully in small portions. 30 min after completed addition, a solution of 1-[2-chloro-4-(2,4-difluorophenoxy)phenyl]ethanone (25 g) in 50 mL THF was added. After stirring overnight, the reaction mixture was diluted with MTBE and sat aq. NH4Cl-Sol was added. The organic phase was separated and the aqueous phase was three times extracted with MTBE (300 mL). the combined organic layers were washed with sat NaHCO3-solution, sat aq. NaCl and dried over Na2SO4. 2-[2-chloro-4-(2,4-difluorophenoxy)phenyl]-2-methyl-oxirane (23.5 g) was obtained as a brown oil and used in the next step without further purification. 1H-NMR (CDCl3; 400 MHz) (ppm)=1.65 (s, 3H); 2.8-3.0 (dd, 2H); 6.75-7.1 (m, 5H); 7.4 (d, 1H).

Provenance & Evidence