HISHICOLIN PX-4MP synthesis

Yield:-

Reaction Conditions:

at 120; for 8 h;Inert atmosphere;

Steps:

1
Under a nitrogen atmosphere, 1.0 mol of tri-n-butyl phosphine (trade name: HISHICOLIN P-4, manufactured by the Nippon Chemical Industrial Co., Ltd.) was mixed with 1.0 mol of trimethyl phosphate (manufactured by Daihachi Chemical Industry Co., Ltd.), and they were allowed to react with each other at 120° C. for 8 hours. The reaction mixture was then cooled to room temperature and sufficiently washed with n-hexane, followed by concentration to give a reaction product. The structure of the reaction product was determined by NMR, and it was confirmed that the reaction product was methyltri-n-butylphosphonium dimethyl phosphate. Further, the purity was found to be 96.40%. Furthermore, the halogen ion content determined by silver nitrate titration was 5 ppm in terms of chlorine.(Test for Light-Transmitting-Properties)The methyltri-n-butylphosphonium dimethyl phosphate obtained as described above was dissolved in acetonitrile to prepare a 0.1M acetonitrile solution, which was then filled into a 1 cm quartz cell to measure the UV absorption-spectrum. The measurement was performed in a wavelength range of 200 nm to 400 mm using a spectrophotometer (U-3400, manufactured by Hitachi, Ltd.) as a measuring apparatus. The result of the measurement is shown in FIG. 1.

References:

NIPPON CHEMICAL INDUSTRIAL CO., LTD. US2010/267980, 2010, A1 Location in patent:Page/Page column 6