HRID868071

反应详情

EQUATION

反应方程式

HRID 868071 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A suspension of 72.4 g (0.16 mole) of 7-[3-t-butoxycarbonylamino-1-pyrrolidinyl]-1-cyclopropyl-6,8-difluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid, 375 ml of 6 M hydrochloric acid, and 750 ml of glacial acetic acid was heated at 60° C. for four hours and the resulting solution was stirred at room temperature for 18 hours. The reaction was filtered through a fiber glass pad to clarify and the filtrate was evaporated in vacuo. The residue was triturated with 600 ml of ethanol:ether (1:1), the solid removed by filtration, washed with ethanol:ether (1:1), ether and dried in vacuo to give 63.8 g (98%) of the title compound, mp 313°-315° C.

WORKUP

后处理

  1. filtrationThe reaction was filtered through a fiber glass pad
  2. customthe filtrate was evaporated in vacuo
  3. customThe residue was triturated with 600 ml of ethanol:ether (1:1)
  4. customthe solid removed by filtration
  5. washwashed with ethanol:ether (1:1), ether
  6. customdried in vacuo