ChemicalBook CAS DataBase List Phenylbis(2,4,6-trimethylbenzoyl)phosphine oxide

Phenylbis(2,4,6-trimethylbenzoyl)phosphine oxide synthesis

9synthesis methods

Product Name:Phenylbis(2,4,6-trimethylbenzoyl)phosphine oxide
CAS Number:162881-26-7
Molecular formula:C26H27O3P
Molecular Weight:418.47

Under nitrogen protection and room temperature, 1.4 g of zinc powder was added to the 100 mL reaction flask with stirring.15 ml of ethyl acetate, 4.1 g of 2,4,6-trimethyl benzoyl chloride, and a solution of 2.5 g of phenylphosphorus dichloride in 5 ml of ethyl acetate was added dropwise to the mixture. After that, the temperature was continued for 2 hours. After the completion of the reaction, 20 mL of water and 1.5 mL of 30% hydrogen peroxide were respectively added to the system, and the reaction was continued for half an hour. Saturated sodium bicarbonate solution was added to neutralize weakly alkaline. Finally, Phenylbis(2,4,6-trimethylbenzoyl)phosphine oxide was obtained after purification.

Phenylbis(2,4,6-trimethylbenzoyl)phosphine oxide

Methanone, 1,1'-(phenylphosphinidene)bis[1-(2,4,6-trimethylphenyl)-

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Yield:162881-26-7 94.7%

Reaction Conditions:

with Nitrogen dioxide in toluene; for 1.5 h;Inert atmosphere;

Steps:

2

Example 2 (3) the reaction flask cooled to 50 ° C, the reaction flask to pass excess nitrogen dioxide gas, stirring the reaction solution to keep the reaction temperature constant, the intermediate product bis (2,4,6 _ - trimethyl (2, 4, 6-trimethylbenzoyl) phenyl phosphine oxide, while generating nitric oxide; passing nitric oxide gas into a gas recovery column, and oxidizing the nitric oxide gas, The tower was filled with enough air to re-oxidize nitric oxide to produce nitrogen dioxide and continue into the reaction bottle for circulation until the reaction is complete; continue stirring for 1.5 hours to complete the reaction and gas spill, stop the reaction, The excess nitrogen dioxide gas with sodium hydroxide solution absorption; (4) The reaction was stopped, separated and extracted, and the organic phase was washed twice with 250 ml of pure water, dried over anhydrous sodium sulfate, The toluene solvent was distilled off under reduced pressure to obtain a yellow target 5) The crude product was recrystallized from hexane to give a light yellow solid, which was 79.2g of the pure product of the target photoinitiator 819. The photoinitiator 819 synthesized by this method was analyzed by PLC for purity over 99.0% Phenyl phosphine dichloride, the yield was 94.7%

References:

CN104151358,2016,B Location in patent:Paragraph 0034; 0037; 0038; 0039