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2-Methylpiperazine → HCID 21473369、化合物

HRID 2293972
ノート
印刷プレビュー

反応式

HRID 2293972 の反応式
[CH2:1]([N:3]1[C:12]2[C:7](=[CH:8][C:9]([F:18])=[C:10](F)[C:11]=2[O:13][CH:14]([F:16])[F:15])[C:6](=[O:19])[C:5]([C:20]([OH:22])=[O:21])=[CH:4]1)[CH3:2].[CH3:23][CH:24]1[CH2:29][NH:28][CH2:27][CH2:26][NH:25]1>N1C=CC=CC=1>[CH2:1]([N:3]1[C:12]2[C:7](=[CH:8][C:9]([F:18])=[C:10]([N:28]3[CH2:27][CH2:26][NH:25][CH:24]([CH3:23])[CH2:29]3)[C:11]=2[O:13][CH:14]([F:16])[F:15])[C:6](=[O:19])[C:5]([C:20]([OH:22])=[O:21])=[CH:4]1)[CH3:2]
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 660572-MethylpiperazineHCID 21473367HCID 21473367、化合物

生成物 1

HCID 21473369HCID 21473369、化合物収率 80.9%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

In 60 ml of pyridine were dissolved 3.19 g (0.01 mole) of 1-ethyl-6,7-difluoro-8-difluoromethoxy-1,4-dihydro-4-oxoquinoline-3-carboxylic acid and 3.0 g (0.03 mole) of 2-methylpiperazine, and the mixture was stirred at 105° to 110° C. for 2 hours. Then, the solvent was removed under reduced pressure. Water was added to the residue, and crystals precipitated were collected by filtration, washed with water and ethanol, and dried to obtain 3.23 g of 1-ethyl-6-fluoro-8-difluoromethoxy-7-(3-methylpiperazin-1-yl)-1,4-dihydro-4-oxoquinoline-3-carboxylic acid as pale yellow powder.

後処理

  1. customThen, the solvent was removed under reduced pressure
  2. additionWater was added to the residue, and crystals
  3. customprecipitated
  4. filtrationwere collected by filtration
  5. washwashed with water and ethanol
  6. customdried

出典と根拠

ORDレコード
ord-1fb2d2224fd642e4a7fccae84a3a6a4f
出典データセット
uspto-grants-1997_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05688791

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート