Ethyl Acetate → HCID 14477681, compound

Participants

Reaction Steps

Ethyl 2-(5-tritylamino-1,2,4-thiadiazol-3-yl)-(Z)-2-hydroxyiminoacetate (60.4 g) was dissolved in dimethyl sulfoxide (210 ml). Potassium carbonate (96.48 g) was added under ice cooling, followed by stirring for 10 minutes. Bromofluoromethane (19 g) was added further, followed by stirring at room temperature for 3 hours. The reaction mixture was added with ethyl acetate (1 l) and washed with water and then with saturated saline. Anhydrous magnesium sulfate was added to the thus-washed reaction mixture to dry the same. The solvent was distilled off, and ethanol (120 ml) was added to the residue. Deposited crystals were collected by filtration and then washed with ethanol to obtain the target product (58.2 g). Infrared spectrum (cm- 1, Nujol) 1735, 1530.

Provenance & Evidence