Methylhydrazine → 4-[1-(t-Butylazo)cyclohexyl]-2-methylthiosemicarbazide

Participants

Reaction Steps

To 10.0 grams (.0434 moles) of 1-t-butylazo-1-isothiocyanatocyclohexane cooled to 5° C. and stirred with a magnetic stirrer in a 50 ml erlenmeyer flask was added 1.99 grams (.0434 moles) of methylhydrazine. The reaction was very exothermic and solids formed immediately. Pentane was added to form a slurry, the reaction mixture stirred for 30 minutes at room temperature and the pentane stripped from the slurry to leave a white solid weighing 10.7 grams (89% crude yield). The product melted at 118°-120° C. with decomposition and its infrared spectrum had a strong band at 1515 cm-1 ##STR22## moderate NH bands at 3225 cm-1 and the isothiocyanate at 2040 cm-1 was absent.

Provenance & Evidence