Researches on morphine. Pt. 1 / by S.B. Schryver and and Frederic H. Lees.

  • Schryver, S. B. (Samuel Barnett), 1869-1929.
Date:
[1900]
Catalogue details

Licence: In copyright

Credit: Researches on morphine. Pt. 1 / by S.B. Schryver and and Frederic H. Lees. Source: Wellcome Collection.

    13/20 (page 1034)
    Bromomorphide is also obtained when morphine is mixed with four or five times its weight of 45 per cent, hydrobromic acid solution, and the whole heated for 2 or 3 minutes over a free flame, until the mix¬ ture begins to darken in colour. The product is then made alkaline with sodium carbonate, and the base extracted with an ether-chloroform mixture. A little unchanged morphine remains undissolved. For preparing large quantities of bromomorphide, the phosphorus tribromide method is the more convenient. The salts of bromomorphide are much more stable than those of the corresponding chloro-compound, and for this reason can be recrystal¬ lised from water with very little loss. They are made by grinding up the base with a slight excess of acid. The hydrochloride, crystallises from water in glistening needles containing 1H20. 0-4545, at 115°, lost 0-0188 H20. H20 = 4-14. Cl7H1802NBr,HCl,H20 requires H20 = 4‘47 per cent. 0-3646 air-dried substance gave 0*3022 mixed AgCl and AgBr. AgCl + AgBr calc. = 0-3 gram. For the determination of the specific rotation, the anhydrous salt obtained by recrystallisation from alcohol was employed. aD= +1°17; 1= 1 dcm. 3 c = 3T57; [a]f°= +41-1°. The liydroibromide is very similar in appearance to the hydrochloride. 0-7492, at 120°, lost 0-0355 H20* H20 = 4-73. 0-2720 air-dried substance gave 0*2242 AgBr. Br = 35*07. C17H1802NBr,HBr,H20 requires H2O = 4*03; Br = 35*77 per cent. • For the determination of the specific rotation a specimen recrys¬ tallised from alcohol was employed : aD= + 1°0'; 1=1 dcm.; c = 2*53; [a]f= +39*5. Deoxymorphine. Chloromorpliide was suspended in about five times its weight of concentrated hydrochloric acid, excess of granulated tin added to the mixture, and the whole heated for 2 or 3 hours on a water-bath. A thick syrup separated out after a time. The liquid was poured off from the undissolved tin, which was then washed several times with hot water to dissolve out all the separated syrup. After filtration, the liquid was saturated with hydrogen sulphide whilst still warm, then corked up, and allowed to stand for some time. The precipitated stannous sulphide is subsequently filtered off and washed with hot water, the washings being added to the filtrate, which is then concen- * Slight decomposition takes place at 120°, the substance becoming somewhat coloured.