2-氟-4-溴甲苯25g(132.3mmol,1.0eq),AIBN 521mg(3.2mmol,0.024eq),Co(OAc)2·4H2O 1.6g(6.5mmol,0.049eq),NaBr 449mg(4.4mmol,0.033eq),溶于HOAc 250mL(10V)中,攪拌全溶待用,將反應(yīng)盤管外浴溫度升至130℃,用氧氣調(diào)節(jié)盤管壓力1.2MPa,進(jìn)而開始打料,體系停留時間1.5h,氧氣3~5eq。將體系直接泵入375mL純化水中,用NaOH固體將體系pH調(diào)至12~14,用125mL MTBE萃取水相兩次,水相再用濃HCl調(diào)pH至1,有大量固體析出,過濾得到目標(biāo)產(chǎn)品25.5g,收率88%。1H-NMR(CDCl3)δ:7.38–7.42(m,2H),7.89(t,1H,J=7.88)。