反応 #1390

ord-a4f5c585a2f143a1af864ac4739e3c74

反応方程式

Cl
hydrochloric acid
Cc1c(F)c(N2CCNCC2)cc2c1c(=O)c(C(=O)O)cn2C1CC1
7-(1-piperazinyl)-1-cyclopropyl-6-fluoro-5-methyl-1,4-dihydro-4-oxoquinoline-3-carboxylic acid
CC(=O)OC(C)=O
acetic anhydride
CC(=O)N1CCN(c2cc3c(c(C)c2F)c(=O)c(C(=O)O)cn3C2CC2)CC1
7-(4-acetyl-1-piperazinyl)-1-cyclopropyl-6-fluoro-5-methyl-1,4-dihydro-4-oxoquinoline-3-carboxylic acid

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    抽出the resultant is extracted with dichloromethane
  2. 2
    乾燥the extract is dried over magnesium sulfate
  3. 3
    濃縮After concentrating
  4. 4
    その他the obtained residue is recrystallized from ethanol

実験手順

To a solution of 7-(1-piperazinyl)-1-cyclopropyl-6-fluoro-5-methyl-1,4-dihydro-4-oxoquinoline-3-carboxylic acid (40 mg) in 5% sodium hydroxide (2 ml) is added acetic anhydride (0.1 ml) at room temperature. After the mixture is made acidic with dilute hydrochloric acid, the resultant is extracted with dichloromethane and the extract is dried over magnesium sulfate. After concentrating, the obtained residue is recrystallized from ethanol to give 7-(4-acetyl-1-piperazinyl)-1-cyclopropyl-6-fluoro-5-methyl-1,4-dihydro-4-oxoquinoline-3-carboxylic acid (29 mg), as white powder, m.p. 261°-263° C.

出典

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