ChemicalBook CAS DataBase List Triphenyl phosphite

Triphenyl phosphite synthesis

7synthesis methods

Product Name:Triphenyl phosphite
CAS Number:101-02-0
Molecular formula:C18H15O3P
Molecular Weight:310.28

1120.5 g (11.90 mol) of phenol (3.3 eq.) are placed in a 3-necked, 3-liter flask filled with nitrogen. 494.0 g (3.60 mol) of phosphorus trichloride is charged into a dropping funnel, and 864.5 g of distilled water is poured into an absorption flask for trapping hydrogen chloride. The reaction mixture is heated in an oil bath to a temperature of 45 ° C with stirring, and phosphorus trichloride is added dropwise over 240 minutes. Next, the reaction mixture is stirred for 20 minutes, heated to a temperature of 70 ° C for 10 minutes, kept at this temperature for 10 minutes, heated to a temperature of 160 ° C for 30 minutes and kept for 1.5 hours. Disconnect and weigh the absorption flask with an aqueous solution of hydrogen chloride and get 1242.0 g of hydrochloric acid (30.4 wt%). Replace the reflux condenser with a distillation nozzle with a once-through cooler and a receiving flask. The reaction flask is heated to a temperature of 170 ° C and maintained for 60 minutes under vacuum at a residual pressure of 300-350 mm RT. Art. Gradually reduce the vacuum to a residual pressure of 10 mm RT. Art. and phenol distillate 149.3 g is collected. After phenol is distilled off, triphenyl phosphite weighing 1091.3 g is obtained.

108-95-2 Synthesis

108-95-2
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$14.00/25g

101-02-0
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$10.00/5g

Yield:101-02-0 94%

Reaction Conditions:

with phosphorus trichloride at 35 - 160; under 7.50075 Torr; for 6 h;Flow reactor;Inert atmosphere;Temperature;

Steps:

1

10 kg of phenol (reactant 1A) was added to the reactor (2). 4.42 kg of phosphorus trichloride (reactant 2B) was pumped to the mixer (5) by metering. The reactor (2) has a temperature of 160 ° C and a pressure of 1 kPag. Phosphorus trichloride (reactant 2B) feed capacity of 1l / h, circulating pump (4) of the circulating flow of 12l / h. The inert gas (C) was charged with a high purity nitrogen gas at a flow rate of 0.5 kg / h and passed through a distributor (3) in a reactor (2). The heat exchanger 2 (8) has a condensing temperature of 35 ° C and the condensate is returned to the top of the column (1). After 6 hours of reaction, the conversion was carried out by gas chromatography, and the conversion of phosphorus trichloride (reactant 2B) was 100% and the yield of triphenyl phosphite (E) was 94%.

References:

CN103724370,2016,B Location in patent:Paragraph 0045; 0046