REPORT FOR MANAGEMENT were already available. Measurements made by or at the request of the funda mental research team gave us a frame work for chemical control of mesoheelol. At this stage the development team took over. At the same time the physical chemistry and analytical re search groups were designing methods for studying stability, for assaying pharmaceutical formulations, and for controlling the final product.
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By this time the pilot plant had built up a supply of intermediates and the final reaction was run. The product passed all chemical controls, in both the pilot plant and control division labora tories, as well as animal safety tests. Mesoheelol was sent on for extensive pharmacological and clinical study. The progress report that carried news of this accomplishment also carried a brief optimistic paragraph from fundamental research about a new discovery, to be known as neoheelol.
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The process controls group was called in when the development team found yield variations apparently unrelated to reaction conditions. After consulta tion, an assay emerged to distinguish the two isomers of a key intermediate. Using this assay it was discovered that the only process controls needed at this point were close pH control of the re action mixture and melting point of the penultimate intermediate. In studying the final hydrogénation to produce mesoheelol, the process controls group devised a simple ultraviolet test to find how much unhydrogenated intermediate remained. The development team confirmed the analysts' finding that the unhydrogenated intermediates could be readily removed by crystallization. As a result, hydrogénation time was cut fi'om 17 hours to 2 hours, leaving 0.5% unhydrogenated to be removed by final recrystallization. The quality standards group was informed of this process change and added a maximum absorption limit at 342 ταμ to ensure removal of this possibly objectionable impurity.
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This fable gives some idea of the functions of the various groups as seen from the pilot plant. For greatest flexibility the pilot plant needs rapid and foolproof methods. But powerful techniques and elaborate apparatus are behind many of the apparently simple tests. Analytical chemists today are com bining the progressive methods of all fields of science with their own tradi tional conservatism. This paper illus trates from the point of view of the pharmaceutical pilot plant how indus try is coming to depend more than ever before on the skill and accurate thinking habits of the modern analytical chemist.
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