(2,4,6-Trimethylbenzoyl)diphenylphosphine oxide

white or cream powder

DryPowder; Liquid; OtherSolid; PelletsLargeCrystals, Liquid

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 (30percent), Low temperature reaction 0.5 hours, After placed at room temperature for mixing, Reaction for 5 hours.After the reaction was completed, 5percent 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 98percent.In 100ml reaction flask was added toluene 32g, 3.45g of sodium metal particles (0.15mol), stirring, dropping 6.9g ethanol (0.15mol) dropwise, the process of maintaining the temperature at 65 ~ 70 ° C.Dropping end, stirring 2h, the reaction system was added dropwise phenylphosphine chloride 33. lg (0.15mol), the control temperature 5 ~ 10 ° C, the dropwise addition is complete, Stirring 1h, continue to the reaction system dropwise 2, 4, 6-trimethylbenzoyl chloride 30.1g (0.16mol), the dropping temperature was controlled at 70 ~ 75 ° C, and then stirred for 5h. The reaction was completed, the reaction material was added 15g of water, stirred lh, standing stratification, the resulting organic phase was adjusted to a saturated aqueous sodium bicarbonate solution pH 7 ~ 8, points to the aqueous phase, the organic phase was washed with water , The resulting organic phase was dehydrated, cooled and crystallized, filtered, Dried to give a pale yellow powdery solid 48.2g, melting point 91 ~ 94 ° C, the liquid content of 99.3percent, a yield of 92.2percent125 g of diphenylphosphine oxide was dissolved in 2 liters of dry tetrahydrofuran, After cooling the ice bath, slowly drop the equivalent amount of butyllithium, The solution was changed from colorless to reddish brown, and the mixture was stirred for half an hour. 150 g of 1, 3, 5-trimethyl-2-trichloromethyl-benzene in 1 liter of tetrahydrofuran was slowly added, Solution red brown slowly faded, the reaction continued to stir for half an hour, TLC detection reaction was completed, 2 liters of saturated solution of sodium bicarbonate was added, extracted with 5 liters of ethyl acetate, the organic phase was dried and the solvent was removed by steaming to give (diphenylphosphonio) (trimethylphenyl) methanone product yield 87percent.70.3 g of benzene (0.90 mol), 48.0 g of aluminum trichloride (0.36 mol), After stirring, 41.2 g of phosphorus trichloride (0.30 mol) was added dropwise thereto.The tail gas is absorbed, the dropping temperature is controlled at about 70° C., and after the drop is completed, the reaction is performed by adding reflux. The maximum reaction temperature is controlled at 120° C. After the reaction is completed, Fall to room temperature. The reaction droplet was slowly added to 240 mL of acid water, and the reaction temperature was controlled to not exceed 20° C. After the dropwise addition, the reaction was continued for 0.5 h. After standing, the aqueous phase and the organic phase were clearly stratified. Both layers were transparent and the organic phase was separated. After washing, 40.0 g of 2, 4, 6-trimethylbenzaldehyde (0.27 mol) are added dropwise to the organic phase.The dropping temperature and the reaction were controlled at 5-10°C. The reaction was monitored by liquid chromatography or thin layer chromatography. After the reaction was completed, a 20percent NaOH aqueous solution was slowly added dropwise to the reaction system to adjust the pH to 2, and 2.74 g of WO3 was added in sequence. 2.0 g tetrabutylammonium bromide, 40.0 g of 30percent hydrogen peroxide water was slowly added dropwise and reacted at this temperature. After the reaction is completed, the mixture is allowed to stand for stratification. The organic phase is washed with saturated saline and 10percent Na2SO3, then the pH is adjusted to neutrality, and finally the solution is desolvated under low pressure. Crystallized from ethyl acetate, filtered, dried and lightened.Step 2: A mixture of 74 g of 1, 3, 5-trimethyl-2-trichloromethyl-benzene and 500 ml of dry THFmixing, Add 9 grams of acid activated magnesium shoulder, Maintain the reaction temperature at 20 degrees Celsius evenly until the magnesium shoulder almost disappeared, DripA solution of 68 grams of freshly distilled diphenylphosphonium chloride in 200 ml of dry THF, The reaction system was stirred at room temperature for 2 hours and then heated to reflux overnight.After the reaction system was cooled to room temperature, Remove most of the solvent, The residue was poured into 1 liter of water, The pH was adjusted between 3-4 with dilute hydrochloric acid and 90 g of a 30percent hydrogen peroxide solution was added with vigorous stirring. The aqueous phase was extracted three times with 400 ml of methylene chloride. The organic phases were combined, dried over magnesium sulfate, filtered, and the solvent was evaporated under reduced pressure. The residue was crystallized from isopropyl ether87 grams of light yellow target compounds pure.

It is a photoinitiator, mainly used in screen printing inks, lithographic printing inks, flexographic printing inks, and wood coatings. TPO can be completely cured on white or high titanium dioxide pigmented surfaces. It is widely used in various coatings. Because of its excellent absorption properties, it is especially suitable for screen printing inks, offset printing, flexographic printing inks, and wood coatings. The coating does not turn yellow, the post-polymerization effect is low, and there is no residue. It can also be used for transparent coating, especially suitable for products with low odor requirements. Used alone in unsaturated polyester containing styrene system, it has high initiation efficiency. For acrylate systems, especially colored systems, usually need to be used in conjunction with amines or acrylamides, and at the same time with other photoinitiators to achieve complete curing of the system. Especially suitable for low yellowing, white systems and thick film layers The curing. The photoinitiator TPO is used with MOB240 or CBP393 to improve the curing efficiency. It is the best extraction solvent for petroleum aromatics equipment, and it is also used as a formylation reagent in the fine chemical industry.

Corrosion inhibitors and anti-scaling agents

Ink, toner, and colorant products

500,000 - 1,000,000 lb

Molecular Weight:348.4
XLogP3:5
Hydrogen Bond Acceptor Count:2
Rotatable Bond Count:4
Exact Mass:348.12791691
Monoisotopic Mass:348.12791691
Topological Polar Surface Area:34.1
Heavy Atom Count:25
Complexity:468
Covalently-Bonded Unit Count:1
Compound Is Canonicalized:Yes