HRID978204

反应详情

EQUATION

反应方程式

HRID 978204 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2.1 g (7.8 mmol) of 1-cyclopropyl-6,7,8-trifluoro-1,4-dihydro-4-oxo-3-quinoline carboxylic acid, 20 ml acetonitrile, 1.2 g (7.8 mmole) 1,8-diazobicyclo[5.4.0]undec-7-ene and 0.7 g (7.8 mmole) of 3-hydroxypyrrolidine was refluxed for 2.5 hours. The reaction was allowed to cool and stirred at room temperature for 48 hours. The resulting precipitate was filtered, washed with diethyl ether, then taken up in isopropyl alcohol. The solid was filtered and washed with ether until dry to give 2.0 g of the title compound, mp 276°-278° C.

WORKUP

后处理

  1. temperaturewas refluxed for 2.5 hours
  2. temperatureto cool
  3. filtrationThe resulting precipitate was filtered
  4. washwashed with diethyl ether
  5. filtrationThe solid was filtered
  6. washwashed with ether
  7. customuntil dry