HRID1759560
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
A mixture containing 7-chloro-1-ethyl-6-fluoro-1,4-dihydro-4-oxo-1,8-naphthyridine-3-carboxylic acid (1.0 g), pyrrolidine (1.31 g), and acetonitrile (80 ml) was heated under reflux for 2 hours. The reaction mixture was concentrated to dryness under reduced pressure. The residue was mixed with 5% hydrochloric acid (25 ml) and the mixture was heated on a steam-bath for several minutes and then cooled. The resulting precipitate was collected, washed with water, and recrystallized from chloroform-ethyl acetate to give 1.0 g of 1-ethyl-6-fluoro-1,4-dihydro-4-oxo-7-(1-pyrrolidinyl)-1,8-naphthyridine-3-carboxylic acid, m.p. 299°-300° C.
WORKUP
后处理
- temperaturewas heated
- temperatureunder reflux for 2 hours
- concentrationThe reaction mixture was concentrated to dryness under reduced pressure
- additionThe residue was mixed with 5% hydrochloric acid (25 ml)
- temperaturethe mixture was heated on a steam-bath for several minutes
- temperaturecooled
- customThe resulting precipitate was collected
- washwashed with water
- customrecrystallized from chloroform-ethyl acetate