By Thomas F. DeRosa
Advances in artificial natural Chemistry and strategies stated in US Patents presents artificial directions for getting ready present and commercially major natural compounds, derivatives, and intermediates as said in issued US Patents. Industries surveyed comprise agrochemical, cosmetics and private care items. each one access includes broad details reminiscent of particular laboratory instructions for getting ready all chemical intermediates and characterization facts. moreover, product optimization experiences, business practise, and new artificial equipment were integrated for chosen entries, in addition to projected examine instructions for destiny product improvement. In Advances in artificial natural Chemistry and strategies suggested in US Patents the author's functional strategy allows readers to spot study and industry tendencies, and remain up to date on present advancements within the box. * presents man made directions for getting ready present and commercially major natural compounds, derivatives, and intermediates as suggested in issued US Patents * Identifies product improvement developments to assist be certain examine components * Elucidates use of the USA Patent and Trademark workplace database
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4-t-Butyl-N-[6-chloro-5-(o-methoxyphenoxy)-2-(4-pyridyl)-4-pyrimidinyl] benzene sulfonamide To a solution of 4,6-dichloro-5-(o-methoxyphenoxy)-2-(4-pyridyl)-pyrimidine (6 g) dissolved in 100 ml THF was added 4-t-butyl benzene sulfonamide potassium salt at ambient temperature and the mixture stirred overnight. The reaction mixture was then poured into 150 ml of water and diethyl ether and the pH adjusted to 5 by the addition of HOAc. Thereupon a precipitate formed and the product isolated by filtration as a beige crystal.
References 1. S. Kuami et al, US Patent 5,093,515 (May 3, 1992) 2. S. Davenport et al, US Patent 4,346,248 (August 24, 1984) 3. M. D. Graves et al, US Patent 6,206,819 (March 27, 2001) Assignee: Rohm and Haas Company Utility: Acetyl Chlorination Catalyst Patent: Reaction i- Formamide, hydrochloric acid, cumene ii- Pridine, n-Butyl ether, thionyl chloride Experimental 1. 062 mol), and cumene (40 g) were refluxed for 1 hour to remove water and then cooled to 120 C. 056 mol) was added and the reaction monitored by gas chromatography until completed.
1 H NMR, IR, and elemental analysis data supplied. 2. 5 ml hydrazine and 7 ml acetic acid added, and the reaction refluxed 2 hours. The mixture was concentrated, the mixture purified by chromatography using neutral alumina and CH2 Cl2 /methyl alcohol, 98:2, and the product isolated in 66% yield. 1 H NMR and elemental analysis data supplied. 3. 086 mmol) was dissolved in 20 ml THF and one drop of a saturated solution of NaOH dissolved in ethyl alcohol and nickel peroxide (51 mg) added. The mixture was stirred over 4 Å molecular sieves for 2 hours, the solution was filtered over a celite pad, and used directly for the next step.