· Py As A Crystalline Solid

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N2 - Transmetalation reactions the place organotin reagents are used for the switch of natural groups to boron halides are among probably the most selective and therefore synthetically helpful strategies for the preparation of organoboranes. We describe right here a uncommon example of the reverse response, where migration of the organic group from boron to tin is promoted by addition of fluoride. The bidentate Lewis acids Fc(BMeR)(SnMe2Cl) (Fc = 1,2-ferrocenediyl; R = phenyl (Ph), thienyl (Th), allyl (All)) react with KF at 45°C to offer the rearranged fluoroboranes Fc(BMeF)(SnMe2R) as oily liquids. With an excess of KF, the fluoroborate complexes K[Fc(BMeF2)(SnMe 2R)] are obtained, which are readily remoted as mild yellow solids in good to excessive yields. For the phenyl derivative it was demonstrated that the borate salt could be transformed back to the fluoroborane by treatment with Me 3SiOTf or addition of pyridine, which gives the adduct Fc(BMeF)(SnMe2Ph) · Py as a crystalline strong. The fluoride and pyridine complexes have been characterized by multinuclear NMR spectroscopy, elemental analysis, and single-crystal X-ray diffraction (for R = Ph). Preliminary mechanistic research recommend an intramolecular process and point out that Lewis acid induced Sn-F bond activation might play an vital role.

The third method of synthesis is began from 2′-carboxy-4 4 1 methylethylidene bis phenol-chlorobenzophenone (21.3.21), and it consists of direct cyclization of the indicated carboxy benzophenone into 3-(41-chlorophenyl)phthalimidine (21.3.29). Subsequent sulfochlorination and amination of this product offers 2-chloro-5-(3-oxo-1-isoindolinyl)-benzolsulfonamide (21.3.29), which is oxidized by varied oxidizers reminiscent of oxygen or hydrogen peroxide in alkaline or chromic acid in acetic acid into chlorothalidone (21.3.26) [51,52].

Instance 8 6-Chloro-4-phenyl-2(1H)quinazolinone 3-Oxide EMI17.1 A mixture of 12.6 g (0.05 mole) of 2-amino-5chlorobenzophenone and 6.Fifty five g (0.055 mole) of phenyl isocyanate was heated on a steam-bath for half-hour, and then 250 ml ethanol and l0.43g (0.15 mole) of hydroxylamine hydrochloride have been added and the mixture was refluxed for two days and then cooled. The strong precipitate that formed was collected on a filter, washed with ethanol, and dried in air to offer 9.42 g (69%) of 6-chloro-4-phenyl-2 (lH)quinazolinone 3-oxide as yellow crystals, m.p. 2672690.

AB - Transmetalation reactions the place organotin reagents are used for the switch of organic groups to boron halides are amongst the most selective and hence synthetically useful strategies for the preparation of organoboranes. We describe here a rare example of the reverse reaction, the place migration of the organic group from boron to tin is promoted by addition of fluoride. The bidentate Lewis acids Fc(BMeR)(SnMe2Cl) (Fc = 1,2-ferrocenediyl; R = phenyl (Ph), thienyl (Th), allyl (All)) react with KF at 45°C to present the rearranged fluoroboranes Fc(BMeF)(SnMe2R) as oily liquids. With an excess of KF, the fluoroborate complexes Ok[Fc(BMeF2)(SnMe 2R)] are obtained, that are readily remoted as gentle yellow solids in good to high yields. For the phenyl derivative it was demonstrated that the borate salt may be converted again to the fluoroborane by remedy with Me 3SiOTf or addition of pyridine, which gives the adduct Fc(BMeF)(SnMe2Ph) · Py as a crystalline stable. The fluoride and pyridine complexes have been characterized by multinuclear NMR spectroscopy, elemental analysis, and single-crystal X-ray diffraction (for R = Ph). Preliminary mechanistic studies counsel an intramolecular process and point out that Lewis acid induced Sn-F bond activation could play an important position.

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