反应详情

To 9.12 grams (.0395 moles) of 1-t-butylazo-1-isothiocyanatocyclohexane cooled to 10° C. and stirred with a magnetic stirrer in a 50 ml erlenmeyer flask was added 2.89 grams (.0395 moles) of diethylamine. The reaction mixture was stirred for 3 hours at room temperature, adding pentane periodically to keep the viscosity low. The pentane was stripped from the reaction mixture to leave a yellow viscous oil weighing 11.4 grams (95% crude yield). The infrared spectrum of the product had a strong broad band at 1520 cm-1 and a sharp NH band at 3300 cm-1 and the isothiocyanate band at 2040 cm-1 was very weak indicating there was a trace of the starting material still present.

1. stirringThe reaction mixture was stirred for 3 hours at room temperature
2. customto leave a yellow viscous oil