The resolution of hyoscine and its components, tropic acid and oscine / by Harold King.
- King, Harold
- Date:
- 1919]
Licence: Public Domain Mark
Credit: The resolution of hyoscine and its components, tropic acid and oscine / by Harold King. Source: Wellcome Collection.
18/34 page 493
![+ 42-84°, the value for the Z-oscinium ion is [M]D — 38’66°, whence [a]D-24-7°. On continuing the fractionation of the mother liquors, 71 per cent, of the Z-oscine ^/-hydrogen tartrate present was isolated in a state of purity. The separation was materially accelerated by inoculation of the less mobile solutions, followed by addition of alcohol in insufficient amount to precipitate an oil. The residual solutions, now relatively rich in <7-oscine ^-hydrogen tartrate, were concentrated to a syrup, and, on allowing to remain in a desiccator exposed to a dehydrating agent, crystallised as a striated mass of crystals. These were collected, freed from the adhering syrupy mother liquor, first by suction and then by very limited use of 50 per cent, alcohol as a washing agent. The salt was a mono- hydrate; and gave [o]D+23'7°. It was recrystallised from water, and separated under similar conditions as a felted mass of needles. These now gave [a]D +27-3° (anhydrous). d-Oscine d-hydrogen tartrate monohydrate melts from 55° to 65°, forming a meniscus at the latter temperature. It readily effloresces when exposed to the atmosphere, and when dehydrated in a vacuum over sulphuric acid loses its water of crystallisation. The anhydrous material still melts at 55—65°. This is probably the melting point of an amorphous form, as, on keeping, it acquires the melting point, of the crystalline anhydrous salt, namely, 163—165° (see below). Three different samples of the salt were analysed for their water content. The first, representing a freshly collected salt, gave the following result: 0-4502, dried over H2S04, lost 0‘0320. H20 = 7T; and a salt which showed some signs of efflorescence gave the following: 0-2023 lost 0-0091. H20 = 4-5. C8H1302N,C4Hc0c,II20 requires H20 = 5‘6 per cent. On keeping for some time, this salt had completely effloresced : 0-1180, dried at 100°, lost nil. 0-1180, dried at 100°, gave 0-2055 C02 and 0'0649 H20. 0 = 47-5; H’=6T5. C8H1302N,C4HP)06 requires 0 = 47-2; 11 = 6-3 per cent. The specific rotation of the dehydrated salt was determined in water: c = 0-949; Z= 2-dcm.; aD+31T'; [a]D + 27‘3°, When the hydrated salt is washed with absolute alcohol, it is transformed into a white, crystalline powder, which is the](https://iiif.wellcomecollection.org/image/b30622074_0018.jp2/full/800%2C/0/default.jpg)
