HRID655271
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureto reflux for 4 h
- washThe mixture was washed with ethyl acetate
- customThe resulting precipitate was collected
- washwashed with water
- customdried in vacuo
- additionTo this solid was added conc
- temperatureH2SO4 (1.2 ml) and MeOH (20 ml) and the solution heated
- temperatureto reflux for 6 h
- temperatureAfter cooling the solvent
- customwas removed in vacuo
- customthe residue purified by flash column chromatography