Acetamide, N,N-diethyl-2,2-difluoro- synthesis

9synthesis methods

Product Name:Acetamide, N,N-diethyl-2,2-difluoro-
CAS Number:686-11-3
Molecular formula:C6H11F2NO
Molecular Weight:151.15

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Yield: 93%

Reaction Conditions:

with potassium fluoride;N-[bis(diethylamino)methylene]-N-ethylethane ammonium fluoride in sulfolane at 200; for 1 h;Solvent;Reagent/catalyst;Temperature;

Steps:

2; 7-8 Example 2
N, N-diethyl-2,2-dichloroacetamide (99%) 1mol,Sulfolane 400ml, N- [bis (diethylamino) methylene] -N-ethyl-ethane ammonium fluoride 0.01mol, potassium fluoride 2mol added to 1000ml equipped with water separator,In a three-necked flask with a reflux condenser, the temperature was raised to 200 ° C and the reaction was carried out for 1 hour.The reaction liquid was detected by gas chromatography. When the content of N, N-diethyl-2,2-dichloroacetamide was reduced to below 0.5%, the reaction was stopped, and the temperature was reduced to about 30 ° C to filter out potassium chloride. The organic phase was The organic phase was distilled under reduced pressure at 50-180 ° C / 20mmHg to obtain 0.93 mol of N, N-diethyl-2,2-difluoroacetamide with a yield of 93%. The remaining primer and catalyst can be recycled.The product N, N-diethyl-2,2-difluoroacetamide was analyzed by gas chromatography, and the purity was 99%.

References:

Ji'ning Kangderui Chemical Technology Co., Ltd.;Chen Junmin;Song Fen;Chen Peigen;Zhang Pinghua;Bi Deyuan CN111056966, 2020, A Location in patent:Paragraph 0030-0032; 00445-0050