HRID2118687

反应详情

EQUATION

反应方程式

HRID 2118687 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 4-hydroxy-3-(2-hydroxyethyl)1-phenyl-1,8-naphthyridin-2-(1H)-one (10 g.) in 30% (v/v) sulfuric acid (200 ml.) was heated to reflux, in an atmosphere of nitrogen, and was held at reflux until no further reaction occured (ca. 5-8 hrs.). After cooling, the solution was added slowly and carefully to an icecooled solution of sodium hydroxide (50% solution; 200 ml.). The mixture was allowed to stand overnight and was then filtered. The product was washed with water, dried in air and recrystallized from dimethylformamide/water, with charcoal treatment, to yield the product, m.p. 276°-277.5° C.

WORKUP

后处理

  1. temperatureto reflux, in an atmosphere of nitrogen
  2. temperatureat reflux until no further reaction
  3. custom(ca. 5-8 hrs.)
  4. temperatureAfter cooling
  5. filtrationwas then filtered
  6. washThe product was washed with water
  7. customdried in air
  8. customrecrystallized from dimethylformamide/water, with charcoal treatment
  9. customto yield the product, m.p. 276°-277.5° C.