HRID342619

反应详情

EQUATION

反应方程式

HRID 342619 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. filtrationThe catalyst was filtered off
  2. concentrationthe filtrate was concentrated
  3. additionThe resulting residue was added with 150 ml of 10% aqueous potassium carbonate
  4. extractionthe mixture was extracted with methylene chloride
  5. customThe organic layer was dried
  6. concentrationconcentrated