Acetic Acid → Oxonorfloxacin

HRID 544221

反応式

HRID 544221 の反応式
[CH2:1]([N:3]1[C:12]2[C:7](=[CH:8][C:9]([F:14])=[C:10](Cl)[CH:11]=2)[C:6](=[O:15])[C:5]([C:16]([OH:18])=[O:17])=[CH:4]1)[CH3:2].[O:19]=[C:20]1[CH2:25][NH:24][CH2:23][CH2:22][NH:21]1.N1C=CC=CC=1.C(O)(=O)C>[OH-].[Na+]>[CH2:1]([N:3]1[C:12]2[C:7](=[CH:8][C:9]([F:14])=[C:10]([N:24]3[CH2:23][CH2:22][NH:21][C:20](=[O:19])[CH2:25]3)[CH:11]=2)[C:6](=[O:15])[C:5]([C:16]([OH:18])=[O:17])=[CH:4]1)[CH3:2]

参加物

6

反応物 4

HCID 176Acetic AcidHCID 1049PyridineHCID 231360Piperazin-2-oneHCID 4831697-Chloro-1-ethyl-6-fluoro-4-oxo-1,4-dihydroquinoline-3-carboxylic acid

生成物 1

HCID 130830Oxonorfloxacin収率 32.4%

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

実験手順

A mixture of 1-ethyl-7-chloro-1,4-dihydro-6-fluoro-4-oxoquinoline-3-carboxylic acid (0.80 g), 2-oxopiperazine (3.0 g) and 4 ml pyridine was heated for 18 hours. The reaction mixture was evaporated under vacuum, an aqueous solution of caustic soda was added to adjust the pH to 10, ice cooled and the undissolved matter was collected and washed with a small amount of an aqueous solution of NaOH. The filtered product was suspended in water, acidified with acetic acid, filtered and washed. The product obtained was dissolved in an aqueous solution of NaOH and acidified with acetic acid. The precipitate was filtered, washed and dried to obtain 0.32 g (32%) of 1-ethyl-1,4-dihydro-6-fluoro-7-(3-oxo-1-piperazinyl)-4-oxoquinoline-3-carboxylic acid.

後処理

  1. temperaturewas heated for 18 hours
  2. customThe reaction mixture was evaporated under vacuum
  3. additionan aqueous solution of caustic soda was added
  4. temperaturecooled
  5. customthe undissolved matter was collected
  6. washwashed with a small amount of an aqueous solution of NaOH
  7. filtrationfiltered
  8. washwashed
  9. customThe product obtained
  10. filtrationThe precipitate was filtered
  11. washwashed
  12. customdried

出典と根拠

ORDレコード
ord-01db1032b51443d88ced429e4e4f1bed
出典データセット
uspto-grants-1984_05
特許番号
US04448962

関連ノート

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