Bases derived from some substituted propenylbenzenes with a note on the preparation of pure methylamine / by T.M. Sharp and W. Solomon.

  • Sharp, Thomas Marvel.
Date:
[1931.]
Catalogue details

Licence: Public Domain Mark

Credit: Bases derived from some substituted propenylbenzenes with a note on the preparation of pure methylamine / by T.M. Sharp and W. Solomon. Source: Wellcome Collection.

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    suggested to us by Mr. J. A. Goodson which is operated as follows. One-tenth of a weighed quantity of the crude methylamine hydro¬ chloride is decomposed by the addition of potassium hydroxide and the liberated bases are absorbed in water in a suitable apparatus. The resulting distillate is added to a cold aqueous solution of the remaining nine-tenths of the material and the gaseous bases are ex¬ pelled by boiling. The process is repeated, one-tenth of the residual solution of hydrochlorides being decomposed for this purpose. On concentrating the solution a product is obtained which does not re¬ spond to the Francis test for ammonia (Compt. rend., 1907,144, 857) and therefore contains less than 0*5% of ammonium chloride. The latter when present in quantities of this order is readily removed from methylamine hydrochloride by recrystallisation from water, as shown by the accumulation of the salt in the resulting mother- liquors, in which it is detectable by the Frangois test. The proportion of the total hydrochlorides to be decomposed at each stage, as well as the number of stages, depends on the purity of the initial material, the procedure described above being suitable for methylamine hydrochloride containing about 5% of ammonium chloride. A product of this quality is obtainable in commerce and by the usual methods of methylating ammonium chloride. The authors wish to express their thanks to Dr. T. A. Henry for his valuable advice and criticism. Their thanks are also due to Messrs. W. A. Cowdrey and A. E. Thursby for assistance with the experimental work, and to Messrs. A. Bennett and H. C. Clarke for a number of microanalyses. They also desire to acknowledge a gift of isoehavibetol from Mr. F. E. Stockelbach of Messrs. Fries Bros., New York. Wellcome Chemical Research Laboratories, London, E.C. 1. [Received, May 2nd, 1931.] Printed in (Jurat Britain bt Richard Clat & Son*. Limitkd. BUN9AT. SUTKOUL