4-CYANO-3-(TRIFLUOROMETHYL)BENZENE-1-SULFONYL CHLORIDE synthesis

Yield:942199-59-9 85%

Reaction Conditions:

with hydrogenchloride;copper(l) iodide;thionyl chloride;sodium nitrite in water;acetone at 0 - 20; for 1 h;Temperature;

Steps:

1-4

Anhydrous cuprous chloride (0.3 g, 0.003 mol, 0.011 eq.) Was added to 500 ml of water, and 80 ml of dichlorosulfoxide was added dropwise under an ice-water bath, and rt overnight to obtain solution a;4-amino-2- (trifluoromethyl) benzonitrile (50.0 g, 0.269 mol, 1.0 eq.)Add 260ml of concentrated hydrochloric acid and 50ml of acetone in an ice water bath.Add sodium nitrite (20.4g, 0.296mol,1.1eq.) Dissolved in 20ml of water, stirred at 0 ° C for 30min,Get reaction solution a;Then add the reaction solution a dropwise to the solution a, and react at room temperature for 30 minutes.TLC monitors for complete response.

References:

CN110407721,2019,A Location in patent:Paragraph 0028-0037