反应详情

250 g (1 mol) of 3,12-diisopropyl-1,2-diaza-1,5,9-cyclododecatriene (diastereoisomeric mixture) is dissolved in 1000 ml of t-butanol in an autoclave with stirrer. After the addition of 25 g of a rhodium/aluminium catalyst (5% by weight of rhodium), hydrogen is injected up to a pressure of 130-150 bars, and hydrogenation is then performed at 150°-180° C. until completion of hydrogen absorption. After cooling, the excess hydrogen is released, the suspension is drawn out by suction, and the catalyst is filtered off through a small amount of "Hyflo" (filtering agent). The filtrate is concentrated in a rotary evaporator, and the product is purified by distillation. There is obtained, as the main fraction, 238 g (94% of theory) of 3,12-diamino-2,13-dimethyltetradecane in the form of colourless oil [b.p. 106°-109° C./0.01 Torr; nD20 =1.4600; IR (liquid) inter alia bands at 3355, 3278 and 1613 cm-1 ].

1. customis then performed at 150°-180° C. until completion of hydrogen absorption
2. temperatureAfter cooling
3. filtrationthe catalyst is filtered off through a small amount of "Hyflo" (filtering agent)
4. concentrationThe filtrate is concentrated in a rotary evaporator
5. distillationthe product is purified by distillation