1,3-Difluorobenzene → Methyl 2,4-difluoro-alpha-oxobenZeneacetate

Participants

Reaction Conditions

Reaction Steps

50 g (0.44 mol) of 1,3-difluorobenzene is dissolved at 20° C. in 135 ml of carbon disulfide with 73.5 g (0.55 mol) AlCl3 and then 55.15 g (0.45 mol) of methyl oxalate chloride is added and the mixture is stirred for 2.5 hours at 20° C. Ice-cold 2 N aqueous hydrochloric acid is added dropwise while cooling, extracted with ethyl acetate; the organic phase is washed with water and 10% aqueous Na2CO3 solution, dried over MgSO4, and evaporated to dryness. Yield: 38.0 g (43% of theory).

Provenance & Evidence