HRID655271

反应详情

EQUATION

反应方程式

HRID 655271 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

(5-Fluoro-quinolin-6-yl)-acetic acid tert-butyl ester (5 g, 19 mmol) in 25 ml of aq. NaOH (4N) was heated to reflux for 4 h. The mixture was washed with ethyl acetate and the aqueous layer was acidified to pH 5 with conc. HCl. The resulting precipitate was collected and washed with water and dried in vacuo to return (5-fluoro-quinolin-6-yl)-acetic acid. To this solid was added conc.H2SO4 (1.2 ml) and MeOH (20 ml) and the solution heated to reflux for 6 h. After cooling the solvent was removed in vacuo and the residue purified by flash column chromatography to return the title compound (2.0 g 48%).

WORKUP

后处理

  1. temperatureto reflux for 4 h
  2. washThe mixture was washed with ethyl acetate
  3. customThe resulting precipitate was collected
  4. washwashed with water
  5. customdried in vacuo
  6. additionTo this solid was added conc
  7. temperatureH2SO4 (1.2 ml) and MeOH (20 ml) and the solution heated
  8. temperatureto reflux for 6 h
  9. temperatureAfter cooling the solvent
  10. customwas removed in vacuo
  11. customthe residue purified by flash column chromatography