The alkaloids of Picralima klaineana, Pierre. Pt. 2 / by T.A. Henry.

  • Henry, Thomas Anderson, 1873-1958.
Date:
[1932]
Catalogue details

Licence: Public Domain Mark

Credit: The alkaloids of Picralima klaineana, Pierre. Pt. 2 / by T.A. Henry. Source: Wellcome Collection.

    12/16 (page 2768)
    OMe, 10-1; NMe, 9-4%). The base persistently gave high carbon results on analysis, due it is believed to slight decomp., which occurs on drying at 100° in vac., the dried product having a faintly brown tinge. On melting, the base and all its salts decompose into a red froth. The picrate forms dark olive- green prisms, m. p. 196°. Non-alkaloidal constituents. As the preliminary extraction of the seeds with light petroleum (p. 2762) proceeds, there accumulates in the flask a greyish- yellow ppt. consisting mainly of wax. This on solution in CHC13 leaves undis¬ solved a small amount of a water-sol. product, which reduces Fehling’s solution on boiling and resembles crude inulin in appearance. The light petroleum extract after removal of the alkaloids' (p. 2762) leaves on evaporation of the solvent a dark greyish-green, semi-solid fat. None of these products has yet been examined in detail. From one sample of seeds from the Belgian Congo, the crude ale. extract, which had been kept for a few days before being worked up, deposited a partly cryst. ppt. This on repeated extraction with EtOH was separated into two portions, the wax already referred to and a sugar. The latter after repeated washing with CHC13 to remove traces of wax was crystallised from aq. EtOH until of const, m. p. 187°. It reduced Fehling’s-solution very slightly before, and copiously after, hydrolysis with boiling HC1. It had [a]p° + 64*84° (c = 3*2 in H20) (Found : C, 41*8; H, 6*45. Calc, for C12H22On : C, 42*1; H, 6*43%). The sugar is therefore sucrose and it showed no depression of m. p. on admixture with that substance. Volatile bases. The residual aq. liquors remaining after pptn. of the total alkaloids developed a slight fishy odour on addition of NaOH. They were therefore steam-distilled after the addition of NaOH, the alkaline steam collected in dilute HCI, and the still acid distillate evaporated to dryness. The residue was re crystallised from H20 in three fractions, which contained respectively 66*25, 66*2, and 65*1% Cl : the portion which did not crystallise from H20 was separated into two more cryst. fractions by trituration first with dry EtOH and finally with Me2CO. These contained 66*1 and 64*2% Cl. In a second instance the crude residue of hydrochloride was fractionated by Goodson’s method (Sharp and Solomon, J., 1931, 1477). The three fractions obtained, representing 25% of the whole and the richest in alkylamine, con¬ tained 66*1, 65*0, and 61*65% Cl (Calc, for NH4C1 : Cl, 66*3. Calc, for CH3NH2,HC1 : Cl, 52*5%). There can be no doubt, therefore, that only a minute amount of alkylamine is present and that NH3 is the chief constituent of the volatile bases. Wellcome Research Institution, London, N.W.l. [Received, September 23rd, 1932.] Printed in Great Britain by Richard Clay & Sons, Limited, BUNGAY, SUFFOLK.