TETRAMETHYL ETHYLENEDIPHOSPHONATE synthesis

Yield:5927-50-4 93%

Reaction Conditions:

with trimethylphosphane in tetrahydrofuran at 0 - 25; for 20.5 h;Catalytic behavior;Schlenk technique;Reagent/catalyst;Solvent;

Steps:

General procedure for PMe₃ catalyzed additionof P(O)-H compounds to vinylphosphorus compounds

General procedure: A glass schlenk tube was charged with P(O)-H compounds (1.0 mmol), vinylphosphorus compounds(1.0 mmol) and 1.0 mL solvent. After the tube was cooled in an ice bath, PMe₃/THF(1.0mol/L, 0.05 L) was injected into it with a syringe. Stirring the mixture for30 minutes, the ice bath was removed and stirring continued for 20 h at room temperature.The reaction was monitored by ³¹P NMR. Removal of the solvent andPMe₃ under reduce pressure gave a crude product which were purifiedby GPC to get the analytically pure samples

References:

Saga, Yuta;Han, Daoqing;Kawaguchi, Shin-Ichi;Ogawa, Akiya;Han, Li-Biao [Tetrahedron Letters,2015,vol. 56,# 38,art. no. 46566,p. 5303 - 5305] Location in patent:supporting information