HRID232039

反应详情

EQUATION

反应方程式

HRID 232039 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 1.4 g (50 mmol) of 1-cyclopropyl-6,7,8-trifluoro-1,4-dihydro-4-oxoquinoline-3-carboxylic acid, 1.92 g (7.5 mmol) of [1-methyl-2-oxo-2-[(3-pyrrolidinyl)amino]ethyl]-carbamic acid 1,1-dimethylethyl ester, 1.5 g (15 mmol) of triethylamine and 75 ml of acetonitrile was heated at reflux for five hours. The solvent was removed in vacuo and the residue was partitioned between chloroform/water (250 ml each) and acidified to pH 2.0 at 0° with 6.0M hydrochloric acid. The solid was removed by filtration, washed with water and dried in vacuo to give 2.4 g of the title compound, mp 185°-187°.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for five hours
  3. customThe solvent was removed in vacuo
  4. customthe residue was partitioned between chloroform/water (250 ml each)
  5. customacidified to pH 2.0 at 0° with 6.0M hydrochloric acid
  6. customThe solid was removed by filtration
  7. washwashed with water
  8. customdried in vacuo