ChemicalBook CAS DataBase List 1,10-DIAMINODECANE

1,10-DIAMINODECANE synthesis

11synthesis methods

Product Name:1,10-DIAMINODECANE
CAS Number:646-25-3
Molecular formula:C10H24N2
Molecular Weight:172.31

1871-96-1
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$20.37/5g

646-25-3
265 suppliers
$6.00/25g

Yield:646-25-3 95%

Reaction Conditions:

with hydrogen;sodium hydroxide in lithium hydroxide monohydrate at 90; under 15001.5 Torr; for 4.25 h;

Steps:

2 Example 2 Sebaconitrile Hydrogenation

Example 2 Sebaconitrile Hydrogenation [0060] 50 g of 1,12-decanediamine and 50 g of water are introduced into a 750-ml autoclave equipped with a self-aspirating turbine. 10 g of Raney nickel doped with 2% by weight of Cr and basified with sodium hydroxide are introduced. The reactor is flushed with nitrogen and then twice with hydrogen, with 10 bar of pressure. Heating is carried out under a hydrogen pressure of 20 bar at 90° C. The sebaconitrile of example 1 is then introduced with a pump; 400 g of dinitrile are injected of the course of 4 hours. The reaction is exothermic. The temperature is kept constant by cooling. After the end of the injection, the mixture is left at 90° C. for 15 min under 20 bar of hydrogen. The mixture is brought back to ambient temperature and the reactor is flushed with nitrogen. The catalyst is filtered off and partially recycled. A catalyst deactivation of 1 g of nickel for 1 kg of hydrogenated dinitrile is accepted. The diamine is then purified by distillation under reduced pressure. The diamine is recovered at 140° C. under 10 mmHg, the latter solidifies at 62° C. The yield is 95%. In order to have a maximum reaction yield, it is necessary to supply the nitrile at a sufficient flow rate without accumulating the nitrile in the reaction medium.

References:

US2013/204001,2013,A1 Location in patent:Paragraph 0060

112-47-0 Synthesis