ChemicalBook CAS DataBase List Phosphonitrilic chloride trimer

Phosphonitrilic chloride trimer synthesis

9synthesis methods

Product Name:Phosphonitrilic chloride trimer
CAS Number:940-71-6
Molecular formula:Cl6N3P3
Molecular Weight:347.66

Hexachlorocyclotriphosphazene (PNCl2)3 (mp114 ℃, bp 256℃), which is produced on an industrial scale as the starting material for the manufacture of organosubstituted polyphosphazenes. It forms an almost planar six-membered ring with equal P?N bond lengths.

Phosphorane, pentachloro-, (TB-5-11)- (9CI)

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Yield:940-71-6 71%

Reaction Conditions:

with pyridine;magnesium chloride in chlorobenzene at 80 - 132;Inert atmosphere;

Steps:

2 In a specific experiment, you can follow the following preparation process:

20.8 g (0.1 mol) of phosphorus pentachloride and 62.4 ml of anhydrous chlorobenzene were added to a 250 ml four-necked flask under nitrogen atmosphere, Slowly raised the temperature to 80 ° C, and stirred at 80 ° C for 1 to 2 hours until the phosphorus pentachloride was completely dissolved and stand-by. 5.88 g of ammonium chloride, 571 mg of magnesium chloride, 474 mg of pyridine and 62.4 ml of anhydrous chlorobenzene were placed in a 250 ml four-necked flask under nitrogen atmosphere, and slowly heated to a reflux state of 130 to 132 ° C under nitrogen atmosphere. The prepared phosphorus pentachloride chlorobenzene solution was slowly added dropwise to a 250 ml four-necked flask under reflux, and the dropping time was controlled to be not less than 4 hours. After the completion of the dropwise addition, stirring was continued under reflux for 1 to 2 hours; After cooling to room temperature, filtration, the mother liquid was concentrated to remove the solvent to obtain a crude compound hexachlorocyclotriphosphazene (referred to as "compound 2").The crude compound 2 obtained above and 10.5 ml of petroleum ether (boiling range 60 to 90) were added to a 50 ml jacketed bottle, Slowly raised the temperature to 80 ° C, stirred at 80 ° C for 1 to 2 hours until the crude product 2 was completely dissolved, and let stand to separate and remove a small amount of oil. The petroleum ether solution was then extracted twice with 40 ml of 98% concentrated sulfuric acid, and the concentrated sulfuric acid extract was diluted to 60% concentrated sulfuric acid solution with 22.7 ml of deionized water to precipitate a crude product of gray hexachlorocyclotriphosphazene. Crude compound 2 and 10.5 ml of petroleum ether (boiling range 60-90) were added to a 50 ml jacketed flask, slowly warmed to 80 ° C, and stirred at 80 ° C for 1 to 2 hours until the product was completely dissolved. Then, the temperature was slowly lowered to 0 to 5 ° C for crystallization, and after filtration, 8.22 g of Compound 2 as white crystals was obtained, yield 71%.The obtained compound was tested and found to be a cyclic hexachloro phosphazene compound having a specific crystal form.

References:

CN109134544,2019,A Location in patent:Paragraph 0221; 0224-0227

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7646-85-7 Synthesis