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

  • Samuel Barnett Schryver
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.

    12/20 page 1033
    porce]ain-like mass is obtained, consisting of a mixture of the base 'with chloroform, from which the chloroform can only be expelled with great difficulty. On the other hand, the base is too slightly soluble in ether for it to be advisable to use this solvent alone. Satisfactory results, however, are obtained by the employment of the ether-chloroform mixture. After extracting four times with a mixture of chloroform and ether, very little of the base remains in the aqueous mother liquors. The chloroform-ether extract is then 'washed four or five times with water to extract the alcohol, rapidly dried with calcium chloride, filtered, and distilled. The base remains behind as a porcelain-like mass with a certain amount of chloro¬ form adhering. On warming for some time on a water-bath with alcohol and then evaporating, a thick syrup is obtained, which is free from chloroform, and solidifies on standing for a short time to a hard mass, which can be readily powdered in a mortar. After drying the powder thus obtained in a water oven, it is further purified by recrystallisation. About 20 grams of base in this crude form are obtained from 20 grams of morphine. In order to purify the product, the only convenient solvent avail¬ able is ether. As, however, it is only slightly soluble in this liquid, it is placed in a Soxhlet apparatus, and extracted for several hours with pure dry ether. It then separates from the ether in hard masses of minute crystals, which are collected, and are quite pure enough for most purposes. A further amount of the base is obtained by concen¬ tration of the ethereal mother liquor. For analysis the substance was recrystallised from ether two or three times. After the first ethereal extraction a certain amount of product remains undissolved. This has not yet been further investigated. As a rule, about 45 grams of recrystallised base are obtained from 60 grams of crude product. Bromomorphide forms a microcrystalline powder of intensely bitter, nauseous taste. It is readily soluble in alcohol or chloroform, but only slightly so in pure dry ether. From benzene or ethyl acetate it sepa¬ rates in a gelatinous form, resembling that obtained from chloroform. It melts at 169—170°. 0-1692 gave 0-3694 C02 and 0*0841 H20. C = 59'5; H = 552. 0-1227 „ 0-2677 C02 „ 0-0622 H20. C = 59-5 ; H = 5-63. 0-5030 „ 18-8 c.c. moist nitrogen at 21° and 763 mm. N = 4*27. 0-3620 „ 0-1904 AgBr. Br = 22-38. 0i7Hi802NBr requires C = 58-62 ; H = 5'17 ; N = 4*02 ; Br = 23*00 per cent. A determination of the specific rotation in methyl alcohol gave the following result: |_a]D = +1°52', J=1 dcm., c = 2-837, [a]if= +65-9°.
    digitised image 1
    digitised image 2
    digitised image 3