HRID1651594

反应详情

EQUATION

反应方程式

HRID 1651594 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 3.8 g (55 mol) of hydroxylamine hydrochloride in 100 ml of water was neutralized by the addition of 55 ml (55 mmol) of 1.0 N sodium hydroxide. To this was added a suspension of 16.5 g (50 mmol) of 7-(3-oxocyclopentyl)-1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxoquinoline acid in a mixture of 150 ml of ethanol and 50 ml (50 mmol) of 1.0 N sodium hydroxide. The reaction mixture was heated at 60° for 4 hours and then at room temperature overnight. The alcohol was removed in vacuo and the aqueous was acidified to pH 2.0 with 6.0 M hydrochloric acid. The solid was removed by filtration, washed with water, and dried in vacuo to give 16.1 g of the title compound.

WORKUP

后处理

  1. additionTo this was added
  2. temperatureThe reaction mixture was heated at 60° for 4 hours
  3. customat room temperature
  4. customovernight
  5. customThe alcohol was removed in vacuo
  6. customThe solid was removed by filtration
  7. washwashed with water
  8. customdried in vacuo