ChemicalBook CAS DataBase List 4,4'-Bis(diethylamino) benzophenone

4,4'-Bis(diethylamino) benzophenone synthesis

8synthesis methods

Product Name:4,4'-Bis(diethylamino) benzophenone
CAS Number:90-93-7
Molecular formula:C21H28N2O
Molecular Weight:324.46

4,4'-Bis(diethylamino) benzophenone can be used as basic dye intermediate,it is synthesised by N1,N1-DIETHYL-4-[4-(DIETHYLAMINO)BENZYL]ANILINE,reaction conditions is dihydrogen peroxide;chloranil;Aliquat 336 in chlorobenzene at 20 - 25.

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Yield:90-93-7 95%

Reaction Conditions:

with 0.3BiCl₃/Silicalite-1 molecular sieve at 25;Reagent/catalyst;Temperature;

Steps:

1.2; 1.3-18; 1-17

(2) Add xBiCl3/Silicalite-1 molecular sieve as a catalyst to the reaction intermediate product obtained in step (1),After that, N,N-diethylaniline was added dropwise, and the temperature was controlled at 25°C for reaction;Wherein, the ratio of the addition amount of N,N-diethylaniline in step (1) to the addition amount of N,N-diethylaniline in step (2) is 1:1.1,The ratio of the molar amount of Lewis acid on the catalyst to the molar amount of solid phosgene added in step (1) is 1:1;(3) The reaction product in step (2) is separated by solid-liquid,The catalyst is recovered to obtain the organic phase, and then the solvent is removed under reduced pressure, the solvent and unreacted N,N-diethylaniline are recovered, and ethanol is used as the recrystallization solvent for recrystallization to obtain tetraethyl Michler's ketone.In this embodiment, in the xBiCl3/Silicalite-1 molecular sieve catalyst, the mass of Silicalite-1 molecular sieve is 100%, and the loading amount x of BiCl3 is 30%. The preparation method is as follows, which specifically includes:The Silicalite-1 molecular sieve was immersed in a 0.5mol/L sodium carbonate aqueous solution for 4 hours, and after solid-liquid separation, it was calcined at 400°C for 5 hours under a helium atmosphere to obtain an activated carrier;The above-mentioned activated support was immersed in a 0.3mol/L BiCl3 solution for 3h, evaporated to remove the solvent at 50°C, and dried in a vacuum to obtain a 0.3BiCl3/Silicalite-1 molecular sieve catalyst.

References:

CN112707830,2021,A Location in patent:Paragraph 0019; 0072; 0075-0148