The resolution of hyoscine and its components, tropic acid and oscine / by Harold King.

  • King, Harold.
Date:
1919]
Catalogue details

Licence: Public Domain Mark

Credit: The resolution of hyoscine and its components, tropic acid and oscine / by Harold King. Source: Wellcome Collection.

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    0*0770 lost 0-0082. H2O = 10*6. 2H20 requires H2O = 10*6 per cent. The anhydrous material consisted of a clear varnish, and had no definite melting point. The melting point of the dihydrate was unchanged after keep- ing in a Jena-glass tube for ten months. d\-Hyosdne Picrate.—This salt was prepared in aqueous solu¬ tion by adding a saturated solution of picric acid to a solution of ^-hyoscine hydrobromide. An oil separated at first, but was dis¬ placed, on warming, by short needles, which melted and decom¬ posed at 173—174°. These were recrystallised from one hundred parts of boiling water, and separated in rosettes of long needles, melting and decomposing at 173-5—174-5° (177*5_178-5° corr.). ’ The same salt is obtained from the d7-base. 61-IIyoscine Aunchloride.—This salt crystallises in long, flat needles with one edge serrated on mixing aqueous solutions of the two components. It melted and decomposed at 214_215°. On recrystallisation from 2’5 per cent, hydrochloric acid, it separated in stout, boat-shaped crystals melting and decomposing at 218—219° (corr.) : 0-1175 gave 0*0358 Au. Au = 30*5. C17H2i04N,AuCl3,HCl requires Au = 30’7 per cent. dl-Hyoscine Auribromide.—On mixing ^-hyoscine hydrobromide dissolved in excess of hydrobromic acid with gold chloride solution, this salt crystallises in chocolate-coloured leaflets of indefinite shape melting and decomposing at 209—210°. On recrystallisation from • )0 parfs of dilute hydrobromic acid solution, it separated in chocolate-red leaflets very similar in appearance to the laevo-sadt. The melting and decomposing point was unchanged at 213_214° (corr.): 0*1123 gave Au = 0-0268. Au = 23’9. 017H2i04N,AuBr3,HBr requires Au = 24*0 per cent. Jowett (loc. cit.) has described a hyoscine auribromide melting at 210°, which probably indicates that his starting material, hyoscine hydrobromide, was optically inactive, or practically so. Hydrolysis of \-Hyoscine. With Hydrobromic Acid.—Pure hydrated ^-hyoscine hvdro- bromide (1*4447 grams), [a]D-22*7° (<r=2*5), was dissolved in 30 c.c. of 10 per cent, hydrobromic acid, and the rotation deter¬ mined. The solution was then boiled gently under reflux, the