| 摘要 |
1,184,949. Ether-diamines. GLANZSTOFF A.G. 17 July, 1967 [2 Aug., 1966], No. 32725/67. Heading C2C. [Also in Division C3] Ether-diamines of formula where R is -O- or O(CH 2 ) n -O- and n is 2 to 4 are prepared and/or purified so that the content of impurities with an OH end group is reduced to less than 1 mole per cent prior to use in the preparation of polyamides (see Division C3). They may be prepared by the conventional process of adding the appropriate glycol to acrylonitrile at 25‹ to 40‹ C. in the presence of aqueous alkali to form the dinitrile, which is then hydrogenated in the presence of Raney cobalt to form the diamine. The desired purity is achieved by (a) extracting the dinitrile intermediate with chlorinated hydrocarbons especially chloroform, and rapidly distilling the extract discarding the first turnings; and (b) effecting the hydrogenation in the presence of solvents or diluents which are completely free from water or alcohol, e.g. benzene, toluene, cyclohexane or tetrahydrofuran. Pyrogallol may also be added to suppress decomposition during the preparation of the dinitrile. Example 1 describes the preparation and purification of ethylene-bis-(3-aminopropyl) ether via ethylene - bis - (2 - cyanoethyl) ether, itself prepared from acrylonitrile and ethylene glycol. The adipic acid salts of ethylene-bis-(3-aminopropyl) ether, the corresponding propylene- and butylene-analogues, and of bis-(3-aminopropyl) ether are also described. |
