HRID2165654

反应详情

EQUATION

反应方程式

HRID 2165654 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A mixture of 2 g of 2-[(1-methylethoxy)methyl]-piperazine, 1.27 g of 1-ethyl-6,7-difluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid and 5 ml of pyridine was heated at 80° C. for 3 hours, then evaporated in vacuo. The residue was reevaporated three times from toluene, giving a gum. Ether was added to the gum which solidified. The solid was triturated with ether containing methanol and then dried giving 2.1 g of solid. A 1 g portion was purified by chromatography, giving 650 mg of the desired product, mp 144°-146° C.

WORKUP

后处理

  1. customevaporated in vacuo
  2. customThe residue was reevaporated three times from toluene
  3. customgiving a gum
  4. customThe solid was triturated with ether
  5. additioncontaining methanol
  6. customdried