2,3,4,4′-Tetrahydroxybenzophenone

Yellow powder

The acylating agent was 0.11 mol of p-hydroxybenzoic acid and 0.1 mol of pyrogallic acid, Concentrated sulfuric acid 0.015 mol was mixed in a reactor, Into the inert gas 10min, When the system temperature rose to 70-80 , Closed reactorAt 110-130 , Pressure 0.1-5MPa, Closed reaction 3h, The reaction was cooled to 50-60 ° C, Insulation 1.5h, Add 20percent ethanol 200ml, Crystallization at 0-5 , Filter drying, To get the product.The molar yield of the product was 78.16percentHPLC ≥ 98.5percent.The acylation reagent p-hydroxybenzoic acid 0.11mol, pyrogallic acid 0.1mol, 0.015 mol of aluminum trichloride and 500 ml of isoamyl alcohol were mixed in the reactor, an inert gas was introduced, When the system temperature was raised to 90-100 , stop the access, continue to heat the reaction at 110-130 for 6h, TLC trace to the end of the reaction, the reaction temperature was cooled to 50-60 , incubated for 1h, Water (100 ml) was added and the layers were separated. The organic layer was crystallized at 0-5 ° C, filtered and dried to give the product.Product molar yield of 78.50percent, HPLC ≥ 98.5percent.The acylation reagent p-hydroxybenzoyl chloride 0.11mol, pyrophilic gallic acid 0.1mol, aluminum trichloride 0.010mol andIsoamyl alcohol 400ml mixed in the reactor, the introduction of inert gas, when the system temperature was raised to 90-100 , stop access, followingContinued heating at 110-130 ° C for 5.5h, TLC trace to the end of the reaction, the reaction temperature was cooled to 50-60 ° C, incubated 1.5h, addWater 200ml, layered, organic layer at 0-5 ° C crystallization, filtration and drying to give the product. The molar yield of the product was 77.20percent, HPLC≥98.5percent.The acylating agent was 0.11 mol of p-hydroxybenzoyl chloride and 0.1 mol of pyrogallic acid, Concentrated sulfuric acid 0.015 mol was mixed in a reactor, Into the inert gas 30min, When the system temperature rose to 70-80 , Closed reactorAt 110-130 , Pressure 0.1-5MPa, Closed reaction 4h, The reaction was cooled to 50-60 ° C, Insulation 2h, Add 20percent ethanol 350ml, Crystallization at 0-5 , Filter drying, To get the product.The molar yield of the product was 72.60percentHPLC ≥ 98.5percent.0.11mol of ethyl p-hydroxybenzoate, 0.1mol of pyrogallic acid, 0.013mol of aluminum trichlorideAnd isoamyl alcohol 450ml mixed in the reactor, the introduction of inert gas, when the system temperature was raised to 90-100 , stop the access, Continue to heat the reaction at 110-130 4.5h, TLC trace to the end of the reaction, the reaction temperature was cooled to 50-60 , incubated 1.5h, Water 150ml was added and the layers were separated. The organic layer was crystallized at 0-5 ° C, filtered and dried to give the product. The molar yield of the product was 73.20percentHPLC ≧ 98.5percent.The acylating agent was 0.11 mol of ethyl p-hydroxybenzoate and 0.1 mol of pyrogallic acid, Concentrated sulfuric acid 0.015 mol was mixed in a reactor, Into the inert gas 30min, When the system temperature rose to 70-80 , Closed reactorAt 110-130 , Pressure 0.1-5MPa, Closed reaction 2h, The reaction was cooled to 50-60 ° C, Insulation 1h, Add 20percent ethanol 300ml, Crystallization at 0-5 , Filter drying, To get the product.The molar yield of the product was 70.80percentHPLC ≥ 98.5percent.Will be acylatedReagents p-hydroxybenzoic acid amine0.09 mol, pyrogallol 0.1 mol, 0.013 mol of aluminum trichloride and 300 ml of isoamyl alcohol were mixed in a reactor, an inert gas was introduced, When the system temperature was raised to 90-100 , stop the access, continue heating at 110-130 reaction 5.5h, TLC trace to the end of the reaction, the reaction temperature was completed to 50-60 , incubated for 1h, Water 200ml was added and the layers were separated. The organic layer was crystallized at 0-5 ° C, filtered and dried to give the product. The molar yield of the product was 70.60percent, HPLC≥98.5percent.In a round bottom flask, pyrogall gallic acid (1.0 mol) was added.P-hydroxybenzoic acid (1.2 mol), Water (700mL), Magnetic silica gel supported imidazolium fluorotitanate (26.0 g), Heating to 90 C, The reaction was stirred for 6 hours.Adsorption by magnetSeparable products and catalysts, Cooling and filtering to obtain a crude product.After washing with water and recrystallization from ethanol, Drying gives the product 2, 3, 4, 4'-tetrahydroxybenzophenone, Yield 88.0%. LC-MS analysis showed that2, 3, 4, 4'-tetrahydroxybenzophenone purity99.4%.The acylating agent was 0.11 mol of p-hydroxybenzoic acid and 0.1 mol of pyrogallic acid, Concentrated sulfuric acid 0.015 mol was mixed in a reactor, Into the inert gas 10min, When the system temperature rose to 70-80 , Closed reactorAt 110-130 , Pressure 0.1-5MPa, Closed reaction 3h, The reaction was cooled to 50-60 C, Insulation 1.5h, Add 20% ethanol 200ml, Crystallization at 0-5 , Filter drying, To get the product.The molar yield of the product was 78.16%HPLC ' 98.5%.The acylation reagent p-hydroxybenzoic acid 0.11mol, pyrogallic acid 0.1mol, 0.015 mol of aluminum trichloride and 500 ml of isoamyl alcohol were mixed in the reactor, an inert gas was introduced, When the system temperature was raised to 90-100 , stop the access, continue to heat the reaction at 110-130 for 6h, TLC trace to the end of the reaction, the reaction temperature was cooled to 50-60 , incubated for 1h, Water (100 ml) was added and the layers were separated. The organic layer was crystallized at 0-5 C, filtered and dried to give the product.Product molar yield of 78.50%, HPLC ' 98.5%.Will be acylatedReagents p-hydroxybenzoic acid amine0.09 mol, pyrogallol 0.1 mol, 0.013 mol of aluminum trichloride and 300 ml of isoamyl alcohol were mixed in a reactor, an inert gas was introduced, When the system temperature was raised to 90-100 , stop the access, continue heating at 110-130 reaction 5.5h, TLC trace to the end of the reaction, the reaction temperature was completed to 50-60 , incubated for 1h, Water 200ml was added and the layers were separated. The organic layer was crystallized at 0-5 C, filtered and dried to give the product. The molar yield of the product was 70.60%, HPLC'98.5%.0.11mol of ethyl p-hydroxybenzoate, 0.1mol of pyrogallic acid, 0.013mol of aluminum trichlorideAnd isoamyl alcohol 450ml mixed in the reactor, the introduction of inert gas, when the system temperature was raised to 90-100 , stop the access, Continue to heat the reaction at 110-130 4.5h, TLC trace to the end of the reaction, the reaction temperature was cooled to 50-60 , incubated 1.5h, Water 150ml was added and the layers were separated. The organic layer was crystallized at 0-5 C, filtered and dried to give the product. The molar yield of the product was 73.20%HPLC ' 98.5%.The acylating agent was 0.11 mol of ethyl p-hydroxybenzoate and 0.1 mol of pyrogallic acid, Concentrated sulfuric acid 0.015 mol was mixed in a reactor, Into the inert gas 30min, When the system temperature rose to 70-80 , Closed reactorAt 110-130 , Pressure 0.1-5MPa, Closed reaction 2h, The reaction was cooled to 50-60 C, Insulation 1h, Add 20% ethanol 300ml, Crystallization at 0-5 , Filter drying, To get the product.The molar yield of the product was 70.80%HPLC ' 98.5%.The acylation reagent p-hydroxybenzoyl chloride 0.11mol, pyrophilic gallic acid 0.1mol, aluminum trichloride 0.010mol andIsoamyl alcohol 400ml mixed in the reactor, the introduction of inert gas, when the system temperature was raised to 90-100 , stop access, followingContinued heating at 110-130 C for 5.5h, TLC trace to the end of the reaction, the reaction temperature was cooled to 50-60 C, incubated 1.5h, addWater 200ml, layered, organic layer at 0-5 C crystallization, filtration and drying to give the product. The molar yield of the product was 77.20%, HPLC'98.5%.The acylating agent was 0.11 mol of p-hydroxybenzoyl chloride and 0.1 mol of pyrogallic acid, Concentrated sulfuric acid 0.015 mol was mixed in a reactor, Into the inert gas 30min, When the system temperature rose to 70-80 , Closed reactorAt 110-130 , Pressure 0.1-5MPa, Closed reaction 4h, The reaction was cooled to 50-60 C, Insulation 2h, Add 20% ethanol 350ml, Crystallization at 0-5 , Filter drying, To get the product.The molar yield of the product was 72.60%HPLC ' 98.5%.Comparative Production Into a three-neck flask, Comparative Production Into a three-neck flask, Production Into a three-neck flask,

Molecular Weight:246.21
XLogP3:2.4
Hydrogen Bond Donor Count:4
Hydrogen Bond Acceptor Count:5
Rotatable Bond Count:2
Exact Mass:246.05282342
Monoisotopic Mass:246.05282342
Topological Polar Surface Area:98
Heavy Atom Count:18
Complexity:298
Covalently-Bonded Unit Count:1
Compound Is Canonicalized:Yes