反应 #443462

反应方程式

4-hydroxybutyric acid

2,3-diaminopyridine

hydrochloric acid

ammonia

→

title compound

收率 66.4%

2-(3-Hydroxypropyl)-3H-imidazo[5,4-b]pyridine

收率 66.4%

反应条件

后处理

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

实验过程

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.

来源