Катализатор межфазного переноса , незаменимая вещь в получении нитрилов

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Embodiment 1:
In the there-necked flask that has electric stirring, thermometer, reflux condensing tube, add acetone 110g, triethylamine 101g and Benzyl Chloride 133g to carry out heated and stirred, reaction rotating speed is controlled at 300～400r/min, 60～66 DEG C of temperature of reaction, reaction times 8～10h, then naturally cool to room temperature, add acetone 202g to dissolve, be then cooled to 5 DEG C, filter, to filter excess dry, obtain triethyl benzyl ammonia chloride, measuring and calculating yield is 86%, and measuring fusing point is 190～191 DEG C.The filtrate that above-mentioned filtration obtains is as reclaiming acetone solvent recycling.
Embodiment 2:
In the there-necked flask that has electric stirring, thermometer, reflux condensing tube, add acetone 110g, triethylamine 101g and Benzyl Chloride 133g to carry out heated and stirred, reaction rotating speed is controlled at 300～400r/min, 60～66 DEG C of temperature of reaction, reaction times 8～10h, then naturally cool to room temperature, add the acetone 202g reclaiming in embodiment 1 to dissolve, be then cooled to 5 DEG C, filter, to filter excess dry, obtain triethyl benzyl ammonia chloride, measuring and calculating yield is 87.5%, measures 190～191 DEG C of fusing points.The filtrate that above-mentioned filtration obtains is as reclaiming acetone solvent recycling.
Embodiment 3:
Acetone 110g, the triethylamine 101g and the Benzyl Chloride 133g that add above-described embodiment in the there-necked flask that has electric stirring, thermometer, reflux condensing tube in, reclaim carry out heated and stirred, reaction rotating speed is controlled at 300～400r/min, 60～66 DEG C of temperature of reaction, reaction times 8～10h, then naturally cool to room temperature, add the acetone 202g reclaiming in above-described embodiment to dissolve, then be cooled to 5 DEG C, filter, to filter excess dry, obtain triethyl benzyl ammonia chloride, measuring and calculating yield is 89.5%, measures 190～191 DEG C of fusing points.The filtrate that above-mentioned filtration obtains is as reclaiming acetone solvent recycling.

 

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1. Ethanol solvent method

Reflex 50.0 g (0.40 mol) of benzyl chloride and 33.7 g (0.33 mol) of triethylamine in 60 ml anhydrous ethanol for 64 hours, cool to room temperature, add 300 ml of ether to precipitate the ammonium salt. Filter, dissolve the ammonium salt in a small amount of hot acetone, add ether for re-precipitation, and obtain the high-purity product.

2. Dimethylformamide solvent method

Reflex 346.5 g of triethylamine, 413.5 g of benzyl chloride, and ethyl acetate in 238.6 g of dimethylformamide (DMF) for 1 hour, then add 300 g of benzene at 80°C to precipitate the ammonium salt. Filter and wash with benzene, then vacuum dry to obtain 648 g of product with a purity of 98.1%.

3. Dichloroethane solvent method

Reflex 23 g of triethylamine and 30 g of benzyl chloride in 120 g of dichloroethane for 2 hours to obtain 52.6 g of Benzyltriethylammonium chloride.

4. Water solvent method

Mix benzyl chloride and triethylamine in a 1:1.2 (mol ratio), stir and reflux for 10 hours using 50-60% aqueous solution of triethylamine. After the reaction, a transparent TEBA aqueous solution with a content of about 60% is obtained, and the yield is 75-85%. Benzyltriethylammonium chloride can be directly used as a catalyst.

5. Solvent-free method

Mix benzyl chloride and triethylamine in a 1:1.3 (mol ratio), fully mix, and place in a stoppered triangular flask. After standing for 60 hours, it solidifies. After recrystallization with petroleum ether, white pure Benzyltriethylammonium chloride is obtained.

 

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