Researches on morphine. Pt. 2 / by S.B. Schryver and Frederic H. Lees.

  • Samuel Barnett Schryver
Date:
[1901]
Catalogue details

Licence: In copyright

Credit: Researches on morphine. Pt. 2 / by S.B. Schryver and Frederic H. Lees. Source: Wellcome Collection.

    12/22 (page 572)
    the fact that the analytical numbers are not in agreement with those required for the formula Cl7H1903N, the presence of alcohol of crys¬ tallisation was suspected. Examination showed that when the crys¬ talline base, previously dried in the steam oven, was heated in an open test-tube to a temperature somewhat above its melting point, alcohol was evolved, which could be ignited at the mouth of the tube. After the evolution of alcohol had ceased, the substance was allowed to cool, when it soon set to a hard, light brown resin ; this was pow¬ dered, dissolved in hot alcohol with the addition of a little animal charcoal, and the solution filtered while hot, when crystals soon separ¬ ated, which were collected and found to exhibit the same behaviour with respect to melting point as the base did before heating. On analysis, the following numbers were obtained: 0-1529 gave 0-3924 C02 and 0 0982 H20. C = 70-0 ; H = 71. 0-6833, heated at 120°, lost 0-0513 C2H60. C2H60 = 7-5. (ClVH1903N)2,C2H60 requires C = 70-1; H = 71 ; C2H60 - 7*4 per cent. Analysis of base free from alcohol : 0-1231 gave 0-3232 C02 and 0 0778 H20. 0 = 71-6; H = 7‘0. Cl7H1903N requires C = 71‘6 ; H = 6*7 per cent. The base when free from alcohol melted sharply at 182°. A deter¬ mination of the specific rotation in methyl alcoholic solution of the base containing -|-mol. of alcohol of crystallisation gave the following result: aD = —3°32'; 1 = 1 dcm.; c = 1*634 ; [a]lT= -216-2°. /3-woMorphine is sparingly soluble in cold, but somewhat more readily in hot, alcohol ; it is almost insoluble in ether or light petrol¬ eum, but readily soluble in hot acetone, benzene, or chloroform ; it also dissolves easily in water, forming a strongly alkaline solution, which almost immediately reduces silver salts. The methiodide was prepared in the usual way. On recrystallisation from water, from which it separated in glistening tablets, it melted at 250° with only slight decomposition. On analysis, the following numbers were obtained : 0-1284 gave 0*2344 C02 and 0-0627 H20. C = 49-8; H = 5-4. 0-4823 required 11*4 c.c. A/10 AgN03 solution. I = 30-0. C^HjgOgNjCHgl requires C = 50*6 ; H = 5*l ; 1 = 29*8 per cent. A determination of the specific rotation in aqueous solution gave the following result : «D= — 3°1T; 1 = 1 dcm. ; c = 2*178 ; [a]~f = -146-1°.