HRID342619
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 suspension containing 18.5 g of ethyl 1-cyclopropyl-6,7-difluoro-1,4-dihydro-8-methyl-5-nitro-4-oxoquinoline-3-carboxylate, 10 ml of Raney nickel, and 300 ml of acetic acid was hydrogenated at room temperature for 1.5 hours under atmospheric pressure. The catalyst was filtered off and the filtrate was concentrated. The resulting residue was added with 150 ml of 10% aqueous potassium carbonate, and then the mixture was extracted with methylene chloride. The organic layer was dried and concentrated to give 14.8 g of pale yellow crystals. The crystals were recrystallized from acetonitrile to give pale yellow needles, m.p. 182.5°-185.5° C.
WORKUP
后处理
- filtrationThe catalyst was filtered off
- concentrationthe filtrate was concentrated
- additionThe resulting residue was added with 150 ml of 10% aqueous potassium carbonate
- extractionthe mixture was extracted with methylene chloride
- customThe organic layer was dried
- concentrationconcentrated