反应详情

温度

90 °C

Into a 300 ml autoclave was placed 10 g of Raney cobalt and 15 g of anhydrous ammonia. A heel of 30 ml of t-butanol was then pumped into the reactor and the reactor heated externally to 90° C. The pressure was then raised to 850 psig with hydrogen. The crude product mixture containing bis(2-cyanoethoxy)ethane and DMAPN from Example 1 was then pumped into the autoclave at a rate of 0.6 g/min until 150 g of the mixture had been admitted. During the addition, the temperature was maintained at 90° C. and the pressure at 850 psig. Following the addition, the reactor was stirred an additional 1 hr until hydrogen uptake was complete. Analysis of the product mixture by GC (t-butanol free basis) revealed the composition to be 21.5 wt % DMAPA. 73.5 wt % of bis(3-aminopropoxy)ethane, 0.72 wt % of 3-aminopropoxyethanol, 1.2 wt % of N-(dimethylamino)-bis(3-aminopropoxy)ethane and 3.1 wt % of bis(aminopropoxyethoxypropyl)amine.

1. additionDuring the addition
2. temperaturethe temperature was maintained at 90° C.
3. additionthe addition