Dimethylcarbamoyl Chloride → HCID 20538681, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 3-t-butyl-5-methylthiopyrazole (6.0 g) and dimethylcarbamoyl chloride (4.3 g) in pyridine (40 ml) were refluxed (at 115° C.) for 16 hours. The pyridine was evaporated, and the residue poured into water and extracted with chloroform. The chloroform layer was washed with 2 N HCl (2×50 ml), then water (50 ml), dried and evaporated to give an oil which soon crystallised. Recrystallisation from 60°-80° petrol at 0° C. gave 5.0 g of 3-t-butyl-1-(dimethylcarbamoyl)-5-(methylthio)pyrazole (59% yield), melting point 56°-8°. Only a single isomer was shown to be present by nuclear magnetic resonance spectroscopy (NMR) and thin layer chromatography.

Provenance & Evidence