Ammonia → HCID 178520526, compound

Temperature

150 °C

0.83 g of 4-hydroxybutyric acid (prepared as described in Preparation 32) was added to 0.77 g of 2,3-diaminopyridine, and the resulting mixture was stirred at 150° C. for 4 hours. At the end of this time, the reaction mixture was treated with 3N aqueous hydrochloric acid and subsequently made alkaline by the addition of aqueous ammonia. The aqueous mixture was evaporated to dryness under reduced pressure, and then the resulting residue was purified by column chromatography through silica gel, using a 5:1 by volume mixture of ethyl acetate and methanol as the eluent. The product was crystallized by trituration with ethyl acetate, to give 0.83 g of the title compound, melting at 151°-153° C.

1. customThe aqueous mixture was evaporated to dryness under reduced pressure
2. customthe resulting residue was purified by column chromatography through silica gel
3. additionby volume mixture of ethyl acetate and methanol as the eluent
4. customThe product was crystallized by trituration with ethyl acetate

ORD record

ord-ff2d3b466b284712a58f7a3e5e4a3e8a

Source dataset

uspto-grants-1998_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05739345