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The preparation of iodine-containing x-ray contrast substances. II. α-phenyl-β-3:s-DI-Iodo-4-Hydroxyphenylpropionic acid (“biliselectan”)

✍ Scribed by Baker, Wilson ;Sansbury, H.


Publisher
Wiley (John Wiley & Sons)
Year
1943
Weight
304 KB
Volume
62
Category
Article
ISSN
0368-4075

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✦ Synopsis


bath (yield 91 g.). The mother-liquor is now concentrnted to nbout 1 litre, filtered after the nddition of charcoal (2 g.), cooled, and the product collected as before (yield 14 6.). Further concentrat.ion of the mother-liquor to about 200 C.C. (1 g, of charcoal) gave another 26. of the compound. The total yield of the purified product is 107 6. It melts with decomposition a t about 247" (liternture 246'), but the melting point rnries somcwhnt with the rate of henting.

3 : 5-Di-iodo-4-pyridone-~-acetic acid is polymorphous. In addition to the form alrendy dcscribed, if hot, fairly concentrated nqueoub solutions nre nlloned to cool slo\vly the bulk of the substnnce separates in thin prismntic needbs, but thick rlmmbic plntcs niny also scpnrnte, nnd these, unlike the otlier forms, bcconie opnque nt 100", and mny be hydrntcd. A further form is obtnined if 0.1 g. is dissolved in 5 c.~. of boiling wntcr nitd set aside; t,his scparntes ns large, flat, irregulnr plntes consisting of braiicliing groitps of crystnls of n fern-like cbnrncter.


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The preparation of iodine-containing x-r
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excessively yith incrensitig pk, cnusing n . consequent high l h i k reading on the instrument3. 4 1 1 view of this i t wns decided to work nt n pII of 4.0, ol)tiiineil iiutoiiint.icnlly by dissolving 0.1 g. of inngncsiuni alloy in 5 nil. of 33% ncetic ncid.