8-Fluorociprofloxacin → PD 135042

HRID 1111459

反応式

HRID 1111459 の反応式
[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

参加物

5

反応物 3

HCID 1228488-FluorociprofloxacinHCID 5360545SodiumHCID 10942334Sodium Methoxide

生成物 1

HCID 465562PD 135042

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.).

後処理

  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)

出典と根拠

ORDレコード
ord-cd9dbbfbebd34aef832b0f06b9b6504a
出典データセット
uspto-grants-1990_12
特許番号
US04980470

関連ノート

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