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ChemicalBook CAS DataBase List Triphenyl phosphate

Triphenyl phosphate synthesis

13synthesis methods
Triphenyl phosphate is prepared by reacting phosphorus pentoxide and phenol (Budavari, 2001), or by reacting phosphorus oxychloride and phenol (Snyder, 1990). On a larger scale phosphorus oxychloride and phenol are reacted in an esterification tank with heating. The HCL formed is trapped and condensed, while the crude triphenyl phosphate runs into a large tank where it is purified.
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Yield:115-86-6 99%

Reaction Conditions:

with 1-methyl-3-(4-((2,4,6-triisopropylphenyl)tellanyl)benzyl)-1H-imidazol-3-ium hexafluorophosphate;Rose Bengal lactone at 15; for 2.5 h;Irradiation;Ionic liquid;Reagent/catalyst;

Steps:

Triphenyl Phosphate (Table 2, Entry 1); Typical Procedure

General procedure: A solution of (PhO)3P (0.0773 g, 0.250 mmol) in (bmim)[PF6] (5mL) containing 5 (0.0330 g, 0.0500 mmol) and rose bengal(0.0128 g, 0.0125 mmol) was vigorously stirred in an open flaskand irradiated with a 60 W LED lamp for 2.5 h. The temperaturewas kept at about 15 °C by using an ice bath during the irradiation.The resulting mixture was extracted with Et2O, and thesolvent was then evaporated to give a pink solid; yield: 0.0803 g(99%); mp 44-47 °C.1H NMR (500 MHz, CDCl3): = 7.36 (t, J = 7.7, 6 H), 7.25-7.19(m, 9 H). 13C NMR (125 MHz, CDCl3): = 150.6, 150.5, 130.0,125.7, 120.3, 120.2. 31P NMR (202 MHz, CDCl3): = -17.7. HRMS(APCI): m/z [M + H]+ calcd for C18H16O4P: 327.0781; found:327.0743.

References:

Mihoya, Aya;Shibuya, Yuga;Ito, Akane;Toyoda, Anna;Oba, Makoto;Koguchi, Shinichi [Synlett,2020,vol. 31,# 20,p. 2043 - 2045] Location in patent:supporting information

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