反応 #1375

ord-b4ccefd875914706b84816f471c88bad

反応方程式

CCOC(=O)c1cn(C2CC2)c2cc(F)c(F)c(C)c2c1=O
ethyl 1-cyclopropyl-6,7-difluoro-5-methyl-1,4-dihydro-4-oxoquinoline-3-carboxylate
Cl
hydrochloric acid
Cc1c(F)c(F)cc2c1c(=O)c(C(=O)O)cn2C1CC1
1-cyclopropyl-6,7-difluoro-5-methyl-1,4,-dihydro-4-oxoquinoline-3-carboxylic acid
収率 92.7%

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度the mixture is refluxed for 2 hours
  2. 2
    温度After cooling
  3. 3
    その他the precipitated crystals are isolated
  4. 4
    洗浄washed with water, ethanol, and diethyl ether in this order

実験手順

To ethyl 1-cyclopropyl-6,7-difluoro-5-methyl-1,4-dihydro-4-oxoquinoline-3-carboxylate (1.9 g) are added 90% acetic acid (20 ml) and conc. hydrochloric acid (5 ml) and the mixture is refluxed for 2 hours. After cooling, the precipitated crystals are isolated, washed with water, ethanol, and diethyl ether in this order to give 1-cyclopropyl-6,7-difluoro-5-methyl-1,4,-dihydro-4-oxoquinoline-3-carboxylic acid (1.6 g), as colorless needles, m.p. 294°-298° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05723648uspto-grants-1998_03