Triethyl Phosphate → [5-(tert-Butyl-diphenyl-silanyloxy)-pent-3-ynyl]-phosphonic acid diethyl ester

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Reaction Steps

A mixture of compound 6 (3.24 g, 80.7 mmol) and triethyl phosphate (40 mL) was refluxed under nitrogen atmosphere for overnight. After evaporation, the residue was purified with 50% EtOAc in hexanes by silica gel column chromatography to give 3.26 g of product 7 (7.90 mmol, 98% yield); 1H NMR (CDCl3) δ 7.77˜7.64 (m, 4H), 7.46˜7.32 (m, 6H), 4.29 (t, J=1.9 Hz, 2H), 4.16˜4.02 (m, 4H), 2.50˜2.34 (m, 2H), 1.96˜1.82 (m, 2H), 1.31 (t, J=7.1 Hz, 6H), 1.04 (s, 9H); 31P NMR (CDCl3) δ 30.43.

Provenance & Evidence