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

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

6synthesis methods

Product Name:Diphenyl(2,4,6-trimethylbenzoyl)phosphine oxide
CAS Number:75980-60-8
Molecular formula:C22H21O2P
Molecular Weight:348.37

487-68-3

4559-70-0

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

75980-60-8

The general procedure for the synthesis of the photoinitiator TPO from 2,4,6-trimethylbenzaldehyde and diphenylphosphine oxide is as follows: 37.61 g of 2,4,6-trimethylbenzaldehyde and 56.17 g of diphenylphosphine oxide were added to a three-necked flask containing 450 ml of methylene chloride, and mixed with stirring. After 6 hours of reaction, the reaction system was cooled in a low temperature water bath to 8?10°C. Subsequently, 0.2925 g of ammonium metavanadate (NH4VO3) and 37 ml of 30% H2O2 were added and reacted at low temperature for 0.5 hours. After that, the reaction mixture was moved to room temperature conditions to continue the reaction for 5 hours. Upon completion of the reaction, 5% aqueous Na2S2O3 was added to the reaction solution to neutralize the unreacted H2O2. Next, an extraction operation was carried out and the organic layer was collected and washed three times with saturated brine. After dehydration by adding anhydrous sodium sulfate, the product was purified by recrystallization. Finally, the product was collected by filtration and dried to give a light yellow powdery solid, the TPO product, in 98% yield.

487-68-3 Synthesis

487-68-3
345 suppliers
$6.00/5g

4559-70-0
332 suppliers
$8.00/5g

75980-60-8
487 suppliers
$14.00/5g

Yield:75980-60-8 98%

Reaction Conditions:

Stage #1: mesytaldehyde;Diphenylphosphine oxide in dichloromethane; for 6 h;Green chemistry;
Stage #2: with ammonium metavanadate;dihydrogen peroxide at 8 - 20; for 5.5 h;Green chemistry;Reagent/catalyst;

Steps:

4 Example 4

37.61 g of 2,4,6-trimethylbenzaldehyde and 56.17 g of diphenylphosphine oxide were added to a three-necked flask with 450 mL of methylene chloride and stirred,Reaction for 6 hours,The three bottles into a low-temperature water bath to cool to 8 ~ 10 ,Followed by adding 0.2925g ammonium metavanadate (NH4VO3), 37mL H2O2 (30%),Low temperature reaction 0.5 hours,After placed at room temperature for mixing,Reaction for 5 hours.After the reaction was completed, 5% Na2S2O3 aqueous solution was added to the filtrate to neutralize the unreacted H2O2,extraction,The organic layer was collected,Washed three times with saturated salt water,Then add anhydrous sodium sulfate in addition to water,Then recrystallized,Suction filtration, drying,A pale yellow powdery solid was obtained,That is TPO products,Yield 98%.

References:

CN106905364,2017,A Location in patent:Paragraph 0030; 0031; 0032; 0033; 0034

707-74-4 Synthesis