8-Fluorociprofloxacin → PD 135042

HRID 1111459

반응식

HRID 1111459 반응식
[CH3:1][O-:2].[Na+].[Na].[CH:5]1([N:8]2[C:17]3[C:12](=[CH:13][C:14]([F:25])=[C:15]([N:19]4[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]4)[C:16]=3F)[C:11](=[O:26])[C:10]([C:27]([OH:29])=[O:28])=[CH:9]2)[CH2:7][CH2:6]1>C(O)C>[CH:5]1([N:8]2[C:17]3[C:12](=[CH:13][C:14]([F:25])=[C:15]([N:19]4[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]4)[C:16]=3[O:2][CH3:1])[C:11](=[O:26])[C:10]([C:27]([OH:29])=[O:28])=[CH:9]2)[CH2:6][CH2:7]1

참가 물질

5

반응물 3

HCID 1228488-FluorociprofloxacinHCID 5360545SodiumHCID 10942334Sodium Methoxide

생성물 1

HCID 465562PD 135042

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To the solution of sodium methoxide prepared from sodium (0.2 g) and absolute ethanol (9 ml) was added 1-cyclopropyl-6,8-difluoro-1,4-dihydro-4-oxo-7-(1-piperazinyl)-3-quinolinecarboxylic acid (0.5 g) and the mixture in sealed tube was heated for 72.5 hours at 140° to 150° C. After cooling, the reaction mixture was concentrated, water (4 ml) was added to the residue, and the solution was adjusted to pH 7 with acetic acid. The insoluble materials were filtered off and the filtrate was allowed to stand in a refrigeretor. The resulting precipitate was collected by filtration and recrystallized from dichloromethane-methanol (2:1; 6 ml) to give the title compound (0.12 g) as colorless prisms, mp 185°-187.5° C. (decompd.).

후처리

  1. temperaturethe mixture in sealed tube was heated for 72.5 hours at 140° to 150° C
  2. temperatureAfter cooling
  3. concentrationthe reaction mixture was concentrated
  4. additionwater (4 ml) was added to the residue
  5. filtrationThe insoluble materials were filtered off
  6. filtrationThe resulting precipitate was collected by filtration
  7. customrecrystallized from dichloromethane-methanol (2:1; 6 ml)

출처 및 근거

ORD 기록
ord-cd9dbbfbebd34aef832b0f06b9b6504a
출처 데이터셋
uspto-grants-1990_12
특허 번호
US04980470

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