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
1-Cyclopropyl-7-(4-oxo-1-piperidyl)-6-fluoro-8-methyl-1,4-dihydro-4-oxoquinoline-3-carboxylic acid (0.25 g) is dissolved in 1% aqueous sodium hydroxide (28 ml), and thereto is added sodium boron hydroxide (0.1 g) at room temperature. The mixture is stirred at the same temperature for 30 minutes, and the resulting mixture is poured into ice water and then acidified with conc. sulfuric acid. The mixture is extracted with dichloromethane, and the solvent is distilled off. The resulting residue is crystallized by adding thereto ethyl acetate, and then recrystallized from chloroform-methanol to give 1-cyclopropyl-7-(4-hydroxy-1-piperidyl)-6-fluoro-8-methyl-1,4dihydro-4-oxoquinoline-3-carboxylic acid (0.16 g), as pale yellow crystals, m.p. 234°-236° C.
WORKUP
后处理
- extractionThe mixture is extracted with dichloromethane
- distillationthe solvent is distilled off
- customThe resulting residue is crystallized
- additionby adding
- customethyl acetate, and then recrystallized from chloroform-methanol