Di-»-butylaminoethyl bromide hydrobromide

The alcoholic ammonia is added to 49 g. (0.16 mole) of di- -butylaminoethyl bromide hydrobromide (Org. Syn. Coll. Vol. 2, 1943, 92) (Note 1) in a 1-1. round-bottomed flask. The flask is stoppered tightly and allowed to stand for six days at room temperature. The solution is then transferred to an evaporating dish and stirred while it is evaporated to a crystalline paste under a hood. The crystalline paste is transferred to a 400-cc. beaker, and to it is added a solution of 16 g. of sodium hydroxide in 18 cc. of water. The solution separates into an upper layer of brown oil arid a lower layer which contains a considerable amount of undis-... 

It is not necessary to isolate the di-w-butylaminoethyl bromide hydrobromide. The crude di- -butylaminoethyl bromide hydrobromide prepared from 405 g. (2.34 moles) of di- -butylaminoethanol is taken up in 600 cc. of water, and the tarry impurities are removed by extraction with three 200-cc. portions of benzene. About 400 cc. of water is evaporated from this solution, and to it is then added 2.8 1. of alcoholic ammonia prepared from absolute ethyl alcohol the concentration of the alcohol in the reaction mixture should be 90 per cent with respect to water. The yield is 114 g. (28 per cent of the theoretical amount based on 405 g. of the aminoethanol). The over-all yield obtained by the procedure described above is 27 per cent, based on the aminoethanol. 

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See also in sourсe #XX -- [ , ]

See also in sourсe #XX -- [ , ]

See also in sourсe #XX -- [ , ]

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