The method of producing benzyldimethylamine

 

(57) Abstract:

The inventive product-benzyldimethylamine, b.F. WITH16H16ABOUT3so pl. 63 - 64oC. Reagent 1: dimethoxymethane. Reaction conditions: at room temperature in the presence of PCl5when the reagent ratio 1:2:PCl51:60:1.

The invention relates to the field of organic chemistry, particularly to a method of producing benzyldimethylamine formula

< / BR>
which can be used as photoinitiator polymerization.

Known methods of obtaining benzyldimethylamine interaction diphenylacetone with idestam the stands and oxide of barium and interaction diphenylacetone with oxide of silver and idestam the stands [1, 2] the Disadvantages of this method is the low yield of the target product.

The closest analogue (i.e., the prototype) is a method of obtaining benzyldimethylamine interaction diphenylacetone with dimethylsulfate and sodium methylate [3] the Process is carried out as follows. To 210 g of diphenylacetone and 177 g of (MeO)2SO2in 800 ml of dioxane for 6 hours stirring and at a temperature of 20oC added 78 g MeONa. The ratio of reagents diphenylacetone:dimethylsulfate:sodium methylate 1 1, 4 1,4 zaderzhivayut at a temperature of 70oC, separate the organic layer is stirred with 1000 ml of water, filtered off the solid product is washed with water, dried in vacuum at 40oC and allocate 246 g benzyldimethylamine, yield 96% tPL61 - 62oC.

It is obvious that the process is sequential, continuous.

The aim of the present invention is to reduce the reaction time and the simplification of the process. This goal is achieved by the interaction of diphenylacetone with dimethoxymethane in the presence petaluridae of phosphorus in a molar ratio 0,05 3 0,05 loaded into the three-neck flask equipped with a mechanical stirrer, thermometer and reflux condenser. Is instant dissolution of diphenylacetone in dimethoxymethane with heat. By neutralizing the reaction mixture with 10% solution of Na2CO3fall white crystals of the product (1). Output 92.94%

Example 1.

In a 3-necked flask with a volume of 0.5 liters, equipped with a mechanical stirrer, thermometer and reflux condenser load 10 g diphenylacetone, 250 ml of dimethoxymethane and portions 10, the Reaction to withstand the weight 20.25 minutes Neutralize 10% R-rum sodium carbonate. Filtered white crystals of benzyldimethylamine,10H).

Example 2.

Analogously to example 1 take 10 g of diphenylacetone, 250 ml of dimethoxyethane and 10 g of PCl5. The yield of the product (1), 11,2

A distinctive feature of the proposed method get is that dramatically reduces the time to perform the reaction, only 20 to 25 minutes (on prototype 24 hours). Not used additional solvents for the reaction are significantly reduced stage of the process. The yield of the target product at the level of a prototype. Thus, the proposed method of synthesis of benzyldimethylamine allows you to:

1. To reduce the reaction time is approximately 50 times.

2. To simplify the technology of obtaining the target product by reducing process steps.

The method of producing benzyldimethylamine processing diphenylacetone meteorous agent, characterized in that as meteorologi agent use dimethoxymethane and the process is conducted in the presence of patalenitsa phosphorus at room temperature in the following ratio of reactants: diphenylacetone:dimethoxymethane:PCl5= 1:60:1, respectively.

 

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1 tbl, 7 ex

FIELD: chemistry.

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11 cl, 2 sch, 1 tbl, 12 ex

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3 cl, 1 dwg, 1 tbl, 1 ex

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15 cl, 19 dwg, 11 tbl, 86 ex

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71 cl, 59 ex

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31 cl, 7 tbl, 8 ex

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,

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used in said methods, as well as use of the compound of formula

, ,

(III), (IV) or (VII) as an intermediate compound in the synthesis of the (E)-stilbene derivative of formula (VI) or polyhydroxystilbene. Values of substitutes R1, R1', R2', R, A, Ar, R' are given in the claim.

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26 cl, 1 dwg, 32 ex

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