HRID542819
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 of 7-fluoro-1-methyl-3-(1-methyl-1H-tetrazol-5-yl)-4-quinolone (5 g) and aqueous sodium hydroxide (5N, 80 ml) was stirred and boiled under reflux for 45 hours. Water (180 ml) was added to the mixture which was then cooled to ambient temperature. The solution was acidified with concentrated hydrochloric acid to pH 4. The resulting precipitate was collected by filtration and washed with boiling industrial methylated spirit (300 ml) and then hot butanol (120 ml). The residue was crystallised from 50% aqueous industrial methylated spirit to give the novel compound 7-hydroxy-1-methyl-3-(1-methyl-1H-tetrazol-5-yl)-4-quinolone, m.p. >320°.
WORKUP
后处理
- temperatureunder reflux for 45 hours
- filtrationThe resulting precipitate was collected by filtration
- washwashed with boiling industrial methylated spirit (300 ml)
- customThe residue was crystallised from 50% aqueous industrial methylated spirit