反应详情

The procedure of Example 1 was followed using tetrabutylpyrophosphate (4 mL, 10.5 mmol) in dry tetrahydrofuran (10 mL), potassium trimethylsilanolate (2.68 g, 21 mmol) in dry tetrahydrofuran (50 mL), and a 24 h reaction time. The product, potassium dibutylphosphate (4.46 g, 90% yield), was isolated as a white solid by concentrating the filtrate under vacuum: 1H NMR (D2O, DSS) δ 0.8-1.05 (dist. t, CH3, 6H), 1.18-1.8 (m, CH2, 8H), 3.74-4.0 (q, CH2, 4H). Anal. Calcd. for C8H18KO4P: C, 38.70; H, 7.31. Found: C, 38.63; H, 7.38.

1. customa 24 h reaction time