HRID729065

反应详情

EQUATION

反应方程式

HRID 729065 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 7-(3-acetamidopiperidin-1-yl)-1-cyclopropyl-6,8-difluoro-1,4-dihydro-4-oxoquinoline-3-carboxylic acid (4.05 g), sodium methoxide (2.16 g) and N,N-dimethylformamide (120 ml) was stirred for 2 hours at 100°-140° C. The reaction mixture was concentrated in vacuumand water was added to the residue. The mixture was neutralized with 1N hydrochloric acid and the neutralized mixture was then concentrated in vacuum. Purification of the concentrated mixture by silica gel column chromatography (chloroform-methanol) gave 7-(3-acetamidopiperidin-1-yl)-1-cyclopropyl-6-fluoro-1,4-dihydro-8-methoxy-4-oxoquinoline-3-carboxylic acid. m.p. 248°-250° C.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated in vacuumand water
  2. additionwas added to the residue
  3. concentrationthe neutralized mixture was then concentrated in vacuum
  4. customPurification of the concentrated mixture by silica gel column chromatography (chloroform-methanol)