Hydrazine, dihydrochloride → HCID 18954842, compound

Participants

Reaction Steps

A solution of 7.15 g (0.0681 mol) of hydrazine dihydrochloride in 95 mL of tert-butanol and 5 mL of water was heated at reflux for 1/2 hour at which time 1.50 g (0.0068 mol) of the product from Step A was added all at once. The reaction mixture was refluxed for 20 hours and the solvent was removed by evaporation under reduced pressure. 200 mL of 1N sodium hydroxide was added and the crude product was extracted with ethyl acetate (3×75 mL). The ethyl acetate was washed with water (100 mL), dried over anhydrous magnesium sulfate, filtered into a flask containing 1.27 g (0.0068 mol) of α,α,α-trifluoro-p-tolylisocyanate. The reaction mixture was stirred at room temperature for 1/2 hour, the solvent was removed under reduced pressure and the crude product was chromatographed using ether/hexanes (35%:65%) as eluent to afford 0.219 g of a white solid; mp 211°-212° C.

Provenance & Evidence