Tetraethyl pyrophosphite

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 5-Chlorosalicylic acid (0.338 g, 1.9 mmol), m-Toluidine (0.2 g, 1.9 mmol) and Tetraethyl pyrophosphite (0.53 g, 2.0 mmol) in dry toluene was refluxed 7 hrs under nitrogen atmosphere. It was diluted with ethyl acetate, washed with HCl (10%) and then with water (3×30 mL). The organic layer was dried (Na2SO4), filtered and evaporated under vacuum. The resulting crude material was purified by column chromatography over SiO2 using mixture of ethyl acetate and hexanes (2:8) to give title compound (0.134 g,) 1H NMR (CDCl3/DMSO-d6) δ 2.38 (s, 3H), 6.89-7.03 (m, 2H), 7.19-7.59 (m, 4H), 8.08 (d, 1H), 9.92 (bs, 1H), 12.05 (s, 1H). was refluxed 7 hrs under nitrogen atmosphere washed with HCl (10%) The organic layer was dried (Na2SO4) filtered evaporated under vacuum The resulting crude material was purified by column chromatography over SiO2 using mixture of ethyl acetate and hexanes (2:8)