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With tert.-butylnitrite; copper(ll) bromide; In acetonitrile; at 20℃; for 1.0h;
PREPARATION 1195-Bromo-2-meth l-oxazole-4-carbonitrileA solution of <strong>[5098-16-8]5-amino-2-methyl-oxazole-4-carbonitrile</strong> (4.0 g, 1.0 eq), CuBr2 (2.0 eq) and tBuONO (2.0 eq) in eCN was stirred at room temperature for 1 hr when starting material was completely consumed. After workup and purification, the title compound was obtained as a tan solid (3.54 g, 58%).
44%
With tert.-butylnitrite; copper(ll) bromide; In acetonitrile; at 20℃; for 1.0h;
To a solution of copper (II) dibromide (544 mg, 2.43 7 mmol) in anhydrous acetonitrile (5 ml) was added tert-butyl nitrite (90%, 112 jil, 1.340 mmol) then the reaction was stirred for 5 mm at ambient temperature. A suspension of <strong>[5098-16-8]5-amino-2-methyl-1,3-oxazole-4-carbonitrile</strong> (150 mg, 1.218 mmol) in anhydrous acetonitrile (2 ml) was added (gas evolution noted) and the deep blue/black reaction mixture was then stirred at ambient temperature for 1 hour. Water (15 ml) was added to give a sky blue solution then EtOAc (15 ml) was added and briefly stirred then the organics were separated, washed with brine, dried over MgSO4, filtered and concentrated in vacuo to yield the title compound as an orange viscous oil (100 mg, 44%).1H NIVIR (500 MHz, Chloroform-d) 2.52 (s, 3H).
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