57090-90-1|(E)-1H-Imidazole-4-carbaldehyde oxime| Ambeed

Yield	Reaction Conditions	Operation in experiment
81%	With acetic anhydride; at 20 - 100℃; for 1h;	(2) Step will be viscous [...] 4 - a hydroxyimino imidazole (0.227 muM), adding acetic anhydride 69.5 g (0.681 muM), the states the dehydration reaction the reaction condition is: 4 - a hydroxyimino imidazole, acetic anhydride molar ratio of 1:3, raising the temperature to 100 C, thermal insulation reaction 1 hours, reduced pressure distillation acetic anhydride, after the end of the distillation, control temperature ? 30 C dropwise 25% of sodium hydroxide aqueous solution to adjust the pH value of 8.0, then adding ethyl acetate extraction twice, extraction layers to mix and then adding 25% sodium chloride aqueous solution washing two times, after washing the oil be reduced pressure distillation ethyl acetate, then adding toluene dehydration, after the completion of the dehydration in toluene on a large number of solid precipitation, filtration, the filter cake and dichloromethane is used for washing, drying to obtain the 17.6g1H - imidazole -4 - carbonitrile content of 97%, yield 81%.
		A 22-L, four-neck, round-bottom flask equipped with a mechanical stirrer, a temperature probe, a condenser, and an addition funnel with a nitrogen inlet was charged with lH-imidazole-4-carboxaldehyde (Aldrich, 1.10 kg, 11.5 mol) and pyridine (3.0 L, 3.0 mol). The reaction flask was cooled to 8 C with an ice bath and hydroxylamine hydrochloride (871 g, 12.5 mol) was added slowly in portions to maintain the internal temperature below 30 C. The reaction was allowed to cool to ambient temperature and stirred for 2 h at ambient temperature. The resulting thick yellow solution was heated to 80 C with a heating mantle and acetic anhydride (2.04 L, 21.6 mol) was added dropwise over 200 min to maintain the temperature below 110 0C during the addition. The reaction EPO <DP n="132"/>mixture was heated at 100 0C for 30 min, after which time it was allowed to cool to ambient temperature and then further cooled in an ice bath. The pH was adjusted to 8.0 (pH meter) by the addition of 25 wt % NaOH (5.5 L) at such a rate that the internal temperature was maintained below 30 C. The reaction mixture was then transferred into a 22-L separatory funnel and extracted with ethyl acetate (6.0 L). The combined organic layer was washed with brine (2 x 4.0 L), dried over MgSO4, filtered, and concentrated to dryness under reduced pressure at 35 0C to give the crude product as a yellow semisolid. The resulting semisolid was suspended in toluene (3.0 L) and stirred for 1 h, after which time it was filtered to give a light yellow solid, which was resuspended in toluene (3.0 L) and stirred for 1 h. The resulting slurry was filtered and the filter cake washed with toluene (2 x 500 mL) to give the title compound as a light yellow solid [870 g, 82%). The 1H and 13C NMR spectra were consistent with the assigned structure.
	With pyridine; acetic anhydride; at 120℃; for 1.5h;	15.0 g (156 mmol) 4-formyl-1H-imidazole in 100 ml of pyridine are combined with 12.5 g (180 mmol) hydroxylamine-hydrochloride at 60 C. with stirring and the mixture is stirred at 60 C. for 1.25 h. Then the mixture is heated to 80 C. and 28.0 ml (297 mmol) acetic anydride are added such that the temperature remains between 80 and 120 C. After removal of the heating bath stirring is continued for a further 1.5 h during the cooling and the mixture is then evaporated down i. vac. The residue is mixed with ice and neutralised with 10n sodium hydroxide solution. The mixture is extracted with ethyl acetate and the combined organic phases are washed with semisat. and sat. sodium chloride solution, dried on magnesium sulphate and evaporated down i. vac. The residue is taken up twice in toluene and in dichloromethane and in each case evaporated down completely. Then the residue is triturated in diethyl ether, filtered and washed with a little diethyl ether and dried. Yield: 12.22 g (127.3 mmol, 82%) C4H3N3 (93.09) Mass spectrum: (M+H)+=94

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CAS No.: 57090-90-1

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CAS No.: 57090-90-1

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[ 57090-90-1 ] Synthesis Path-Downstream 1~2

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