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