반응 #1390

ord-a4f5c585a2f143a1af864ac4739e3c74

반응 방정식

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

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출the resultant is extracted with dichloromethane
  2. 2
    건조the extract is dried over magnesium sulfate
  3. 3
    농축After concentrating
  4. 4
    기타the obtained residue is recrystallized from ethanol

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05723648uspto-grants-1998_03