反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
Chemistry FIG. 11 illustrates the synthesis of diphosphitylating and triphosphitylating reagents (6 and 7). Phosphorus trichloride (21, 20 mmol) was reacted with 3-hydroxypropionitrile (22, 1 eq) to yield 2-cyanoethylphosphorodichloridite (23). The subsequent reaction of 23 with diisopropylamine (20 mmol, 1 eq) afforded 2-cyanoethyl diisopropylphosphoramidochloridite (24). Addition of water (1 eq) gave the intermediate 25 that was reacted with 24 (1 eq) or 23 (0.5 eq) to yield the diphosphitylating (26, 97%) and triphosphitylating (27, 94%) reagents, respectively. The chemical structures of 26 and 27 were determined by nuclear magnetic resonance spectra (1H NMR, 13C NMR, 31P NMR) and high-resolution time of flight electrospray mass spectrometry. Stability studies using spectroscopic methods showed that the compounds remained stable even after two weeks storage at −20° C.