Name:3-methylbut-2-en-1-yl phosphate
Chemical Formula: C5H9O4P2-
Molecular Weight: 164.0979
m/z: 82.0124 (100.0%), 82.5141 (5.4%)
Elemental Analysis: C, 36.60; H, 5.53; O, 39.00; P, 18.88
参考路线:
参考步骤:
General procedure: To a solution of the alcohol (1 mmol) in acetonitrile (1 mL), trichloroacetonitrile (2.4 mmol) is added, followed by dropwise addition of tetrabutylammonium dihydrogenphosphate (2.0 mmol) in acetonitrile (5 mL). The reaction mixture is stirred at room temperature for two hours, or until all the starting material is consumed. The solvent is removed in vacuo and the crude material is pre-purified by flash chromatography on silica gel (isopropanol/conc. aq NH4OH/H2O 7:2:1). The column fractions which show the presence of phosphate on TLC (e.g., with molybdate reagent) are combined and concentrated under reduced pressure. A Dowex 50WX8 ion-exchange column of 8 cm tall and 1 cm diameter is loaded and equilibrated with a mixture of conc. NH4OH/H2O 3:1 and afterward flushed with a buffer solution of 0.025 M NH4HCO3 until the pH reaches 8.0. The silica column residue is percolated through the DOWEX column with the same NH4OH buffer, collected, and dried either by lyophilization or by evaporation under reduced pressure until excess ammonium hydrogen carbonate is evaporated. The residual ammonium organophosphates are isolated as white solids