ChemicalBook CAS DataBase List Ethyl (2,4,6-trimethylbenzoyl) phenylphosphinate

Ethyl (2,4,6-trimethylbenzoyl) phenylphosphinate synthesis

10synthesis methods

Product Name:Ethyl (2,4,6-trimethylbenzoyl) phenylphosphinate
CAS Number:84434-11-7
Molecular formula:C18H21O3P
Molecular Weight:316.33

0.1 mol phenylphosphinic acid and 100 mL chlorobenzene were added to the reaction vessel. 0.11 mol 2,4,6-trimethylbenzaldehyde was added dropwise under controlled temperature, followed by 2 hours of incubation at 100-120°C. After cooling, pH was adjusted to 4-6 with hydrochloric acid, then 0.13 g vanadium acetylacetonate was added as a catalyst. 0.15 mol of 35% hydrogen peroxide was added dropwise at a rate of 5-10 drops per minute, with the mixture insulated at 5-10°C. The reaction was monitored by TLC until completion.
The reaction mixture was diluted with 100 mL water, neutralized with saturated sodium bicarbonate, and the organic layer was separated and washed twice with water. Excess oxidant was reduced with aqueous sodium sulfite, and the organic layer was separated and washed again. The mixture was dehydrated with anhydrous sodium sulfate, filtered to remove the desiccant.
To the dehydrated organic layer, 0.11 mol sodium hydroxide was added, followed by dropwise addition of 0.55 mol diethyl sulfate at 60-80°C. After the reaction was complete, the mixture was adjusted to pH 8-10 with sodium hydroxide, washed with water, and the organic layer was separated. The organic layer was dried over anhydrous sodium sulfate, filtered, and the solvent was evaporated under reduced pressure to yield Ethyl phenyl(2,4,6-trimethylbenzoyl)phosphinate.

1754-49-0 Synthesis

1754-49-0
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938-18-1 Synthesis

938-18-1
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$9.00/25g

Ethyl (2,4,6-trimethylbenzoyl) phenylphosphinate

84434-11-7
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Yield:84434-11-7 328 kg

Reaction Conditions:

with triethylamine at 75; for 2 h;Large scale;

Steps:

4 Arylphosphine oxide section

The ethyl diphenylphosphonite is continuously input into the high-level dripping tank under negative pressure,In a temperature zone around 75 degrees Celsius, dropwise add to the acylphosphine oxygen synthesis kettle pre-mixed with 230 kg of 2,4,6-trimethylbenzoyl chloride and 8 kg of triethylamine.The reaction is completed in about 2 hours, and the chloroethane gas generated during the process is input into the condensation recovery device under the protection of static electricity.26 kg of dilute hydrochloric acid was added to the reaction solution to remove residual acid chloride, 1000 liters of toluene were pumped in, and the reaction was stirred to obtain a homogeneous liquid.Put the reaction liquid into the washing tank from the bottom valve of the synthesis tank,The temperature is controlled at about 50 degrees Celsius, and the reaction solution is washed with alkaline water, acid water, and neutral water in sequence.The organic phase is automatically input into the vacuum desolventizing kettle, the temperature is controlled not to exceed 75 degrees Celsius, and the toluene solvent is recovered.After adding 700 liters of ethanol to the residue, it was heated with activated carbon to decolorize, and the reaction solution was filtered while it was hot.The ethanol is removed to obtain 328 kg of TPO-L light yellow liquid product (purity above 96%).

References:

CN112778360,2021,A Location in patent:Paragraph 0075-0076