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1-Methylpiperazine → 7-Fluoro-8-(4-methyl-1-piperazinyl)-5-oxo-1,2-dihydro-5H-thiazolo (3,2-a)-quinoline-4-carboxylic acid

HRID 2295719
ノート
印刷プレビュー

反応式

HRID 2295719 の反応式
Br[C:2]1[CH:11]=[C:10]2[C:5]([C:6](=[O:18])[C:7]([C:15]([OH:17])=[O:16])=[C:8]3[S:14][CH2:13][CH2:12][N:9]32)=[CH:4][C:3]=1[F:19].[CH3:20][N:21]1[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]1>N1C=CC=CC=1>[F:19][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:2]=1[N:24]1[CH2:25][CH2:26][N:21]([CH3:20])[CH2:22][CH2:23]1)[N:9]1[CH2:12][CH2:13][S:14][C:8]1=[C:7]([C:15]([OH:17])=[O:16])[C:6]2=[O:18]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 531671-MethylpiperazineHCID 131164168-bromo-7-fluoro-5-oxo-1,2-dihydro-5H-thiazolo(3,2-a) quinoline-4-carboxylic acid

生成物 1

HCID 100672737-Fluoro-8-(4-methyl-1-piperazinyl)-5-oxo-1,2-dihydro-5H-thiazolo (3,2-a)-quinoline-4-carboxylic acid収率 22%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A mixture of 500 mg (1.45 mmol) of 8-bromo-7-fluoro-5-oxo-1,2-dihydro-5H-thiazolo(3,2-a) quinoline-4-carboxylic acid, 730 mg (7.25 mmol) of N-methylpiperazine and 10 ml of pyridine was heated to reflux for twelve hours on an oil bath. The conent was then concentrated under reduced pressure, water was added to the residue, insoluble matters were collected by filtration, washed with water, dried, and the resulting powder was recrystallized from dimethyl formamide to give 116 mg (22.0 percent) of the title compound. Melting point was 267° to 271° C. (decomposition).

後処理

  1. temperaturewas heated
  2. temperatureto reflux for twelve hours on an oil bath
  3. concentrationThe conent was then concentrated under reduced pressure, water
  4. additionwas added to the residue, insoluble matters
  5. filtrationwere collected by filtration
  6. washwashed with water
  7. customdried
  8. customthe resulting powder was recrystallized from dimethyl formamide

出典と根拠

ORDレコード
ord-06c50cd67bf0499dac6fd380f90164ca
出典データセット
uspto-grants-1984_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04426381

反応ノート

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