Difluoroacetic acid → HCID 14551036, compound

Participants

Reaction Steps

Difluoracetic acid was added to a mixture of carbonyl diimidazole (8.4 g, 0.052 mol) and methylene chloride (100 ml) under a nitrogen atmosphere. Gas was evolved and a new solid formed in the reaction. After stirring at room temperature for 30 minutes, 5-amino-2-methoxypyridine (5.7 ml, 0.052 mol) was added over a two-minute period. The reacion was slightly exothermic and was stirred further for another 30 minutes when it was washed with water (100 ml), 5% aqueous acetic acid (2×50 ml), 5% sodium bicarbonate (25 ml); dried over anhydrous magnesium sulfate; filtered; and evaporated in vacuo to give an oil. The oil was extracted with ether and the ether extract on dilution with pentane gave 3.7 g of crude product. This was extracted with ether and diluted with pentane to give 2.0 g of the title compound, m.p. 75°-78° C. The title product was identified by IR, NMR and MS analysis.

Provenance & Evidence