反应详情

温度

100 °C

A mixture of 1-(chloromethyl)-2-fluoro-5-methoxy-4-nitrobenzene (Compound 130C, 1.578 g, 7.186 mmol) and triethyl phosphite (1.43 g, 8.62 mmol) was heated at 100° C. for 16 h in a sealed tube. After concentrating the reaction mixture under reduced pressure, the crude product was purified by silica gel chromatography on an ISCO combi-flash system using DCM/MeOH as eluent (100:0→95:5) to give an orange oil, 800 mg (35% yield). 1H NMR (CDCl3, 400 MHz): δ=1.30 (t, J=7.07 Hz, 6 H), 3.20-3.27 (m, 2 H), 3.97 (s, 3 H), 4.11 (dd, J=8.08, 7.07 Hz, 4 H), 7.17 (dd, J=5.94, 2.65 Hz, 1 H), 7.67 (dd, J=8.72, 0.88 Hz, 1 H). MS (ES+): m/z 322.09 [MH+] (TOF, polar).

1. concentrationAfter concentrating the reaction mixture under reduced pressure
2. customthe crude product was purified by silica gel chromatography on an ISCO combi-flash system
3. customto give an orange oil, 800 mg (35% yield)