2,6-DIFLUOROBENZYL MERCAPTAN synthesis

Yield:326829-04-3 45%

Reaction Conditions:

with potassium carbonate in N,N-dimethyl-formamide at 20; for 168 h;Conversion of starting material;

Steps:

I42

2,6-Difluorbenzylthiol (0.33 g, 2 mmol) and potassium carbonate (1.84 g, 13mmol) were added to a solution of 3-chloro-5,5-dimethylisoxazoline (0.26 g, 2 mmol) indry DMF (7.5 ml) under nitrogen. The mixture was stirred for 5 hours at roomtemperature and stored at room temperature for 1 week. The mixture was filtered and thefiltrate diluted with water. The aqueous phase was extracted with ethyl acetate twice. Thecombined organic extracts were washed with water and brine, dried over magnesiumsulfate and concentrated. The crude product was purified by chromatography on silica gel(eluent: ethyl acetate / hexane) to give the product as a white solid (0.23 g, 45% yield).

References:

WO2006/24820,2006,A1 Location in patent:Page/Page column 137