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ChemicalBook CAS DataBase List Diphenyl phosphate
838-85-7

Diphenyl phosphate synthesis

11synthesis methods
-

Yield:838-85-7 71%

Reaction Conditions:

with 1-Butylimidazole;phosphoric acid;triethylamine in N,N-dimethyl-formamide at 230; for 24 h;Inert atmosphere;Temperature;Reagent/catalyst;

Steps:

General procedure for the synthesis of diaryl phosphates

General procedure: Phosphoric acid 85% (461.2 mg, 4.0 mmol), phenol (3.76 g, 40 mmol), triethylamine (1.21 g, 12 mmol), 1-butylimidazole (149.0 mg, 1.2 mmol) and DMF (5 mL) were placed in the reaction apparatus consisted of a 50 mL three-necked flask with a tube through which the boiling solvent and water vapor flowed and a tube through which the solvent was refluxed through the dehydrating agent. (See Fig. S1) PAdeCS, 2.0 gram as a drying agent is put under the condenser. The reaction was heated at 230 °C for 24 h and after this time, the resulting mixture was run through cation exchange resin (eluent: MeOH) to remove amines. After evaporation of eluent, the mixture was distilled at low pressure to remove phenol and DMF. The desired diphenyl hydrogen phosphate is obtained by gel permeation chromatography GPC (eluent: CHCl3), 71% (619.6 mg, 2.84 mmol).

References:

Tran, Cong Chi;Asao, Kazuya;Sasaki, Takeshi;Hayakawa, Yasuyuki;Kawaguchi, Shin-ichi [Tetrahedron Letters,2022,vol. 96,art. no. 153726] Location in patent:supporting information

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