反应详情

温度

100 °C

A mixture of 4-(chloromethyl)-2-methoxy-1-nitrobenzene (1.1 g, 5.46 mmol) and diethyl methylphosphonite (0.89 g, 1.2 mmol) were heated at 100° C. for 16 h in a sealed tube. The reaction mixture was concentrated in vacuo and the residue crude purified using an Isco Combiflash system eluting with 0→5% MeOH in DCM as eluent to afford 0.641 g of ethyl (3-methoxy-4-nitrobenzyl)methylphosphinate (yield: 43% yield). MS (ES+): m/z 273.99 [MH+] (ZQ3, polar 5 min).

1. concentrationThe reaction mixture was concentrated in vacuo
2. customthe residue crude purified
3. washeluting with 0→5% MeOH in DCM as eluent