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ChemicalBook CAS DataBase List Diphenylphosphinic Chloride
1499-21-4

Diphenylphosphinic Chloride synthesis

14synthesis methods
To an oven-dried 100 mL, a two-necked flask fitted with a reflux condenser was added Et2O (depending on the Grignard reagent solution's concentration) and POCl3. The solution was cooled in an ice-salt mixture, and a Grignard reagent solution in Et2O was slowly added. After stirring with cooling for 30 min, the reaction mixture was brought to rt and stirred for the indicated time. The mixture was then cooled in an ice-salt mixture, and the alcohol and pyridine were slowly added. Stirring with cooling for 5 min was followed by reaction at rt. The reaction was quenched after the indicated time by cooling in an ice-salt mixture and adding sat aq NH4Cl. The crude mixture was then poured into CH2Cl2, washed three times with HCl, dried, filtered, and evaporated to dryness. The excess alcohol was removed using a short-path vacuum distillation apparatus, and the resulting crude product Diphenylphosphinic Chloride was purified by column chromatography.Diphenylphosphinic Chloride
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Yield:1499-21-4 233 kg

Reaction Conditions:

with phosphorus at 340 - 360; for 4 h;Inert atmosphere;Large scale;Reagent/catalyst;Temperature;

Steps:

1-4 Aryl phosphine halide section

Place 66 kg of yellow phosphorus in a pressure-resistant reactor under the protection of nitrogen.Add 375 kilograms of chlorobenzene and 190 kilograms of phenylphosphinic dichloride from the automatic metering infusion tank,The mixture is heated to 340-360 degrees Celsius for 4 hours under airtight pressure. After the reaction system is cooled to room temperature,The obtained liquid mixture is directly automatically input into the distillation kettle, and the fractional distillation device is turned on.First, distill under normal pressure to obtain a mixture of about 90 kg of chlorobenzene and phosphorus trichloride (recovered and applied),Then vacuum distillation was collected to obtain 235 kg of phenylphosphinic dichloride (recovered) and 233 kg diphenylphosphinic chloride.

References:

CN112778360,2021,A Location in patent:Paragraph 0070-0076

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