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Ethyl 6,7-difluoro-8-methoxy-4-oxo-1-(2,2,2-trifluoroethyl)-1,4-dihydroquinoline-3-carboxylate → 6,7-Difluoro-8-methoxy-4-oxo-1-(2,2,2-trifluoroethyl)-1,4-dihydroquinoline-3-carboxylic acid

HRID 251850
ノート
印刷プレビュー

反応式

HRID 251850 の反応式
[F:1][C:2]1[CH:3]=[C:4]2[C:9](=[C:10]([O:13][CH3:14])[C:11]=1[F:12])[N:8]([CH2:15][C:16]([F:19])([F:18])[F:17])[CH:7]=[C:6]([C:20]([O:22]CC)=[O:21])[C:5]2=[O:25]>C(O)(=O)C.O.S(=O)(=O)(O)O>[F:1][C:2]1[CH:3]=[C:4]2[C:9](=[C:10]([O:13][CH3:14])[C:11]=1[F:12])[N:8]([CH2:15][C:16]([F:19])([F:17])[F:18])[CH:7]=[C:6]([C:20]([OH:22])=[O:21])[C:5]2=[O:25]
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 57794119Ethyl 6,7-difluoro-8-methoxy-4-oxo-1-(2,2,2-trifluoroethyl)-1,4-dihydroquinoline-3-carboxylate

生成物 1

HCID 577941896,7-Difluoro-8-methoxy-4-oxo-1-(2,2,2-trifluoroethyl)-1,4-dihydroquinoline-3-carboxylic acid

試薬・触媒・溶媒 1

HCID 86597087Acetic acid sulfuric acid water溶媒

実験手順

800 mg (2.19 mmol) of the compound of Example 23A are provided in a mixture of 25 ml of acetic acid-water-sulfuric acid 12:8:1 and stirred over night under reflux. For the work-up the solvent is removed to a large extent on a rotary evaporator, the residue is adjusted carefully to pH 3 while cooling with ice with a saturated sodium hydrogen carbonate solution, the suspension is diluted with water, the precipitate is collected by suction filtration and after drying the filter residue under high vacuum, 575 mg of the title compound are obtained.

後処理

  1. temperatureunder reflux
  2. customFor the work-up the solvent is removed to a large extent on a rotary evaporator
  3. temperaturewhile cooling with ice with a saturated sodium hydrogen carbonate solution
  4. additionthe suspension is diluted with water
  5. filtrationthe precipitate is collected by suction filtration
  6. dry with materialafter drying the filter residue under high vacuum, 575 mg of the title compound
  7. customare obtained

出典と根拠

ORDレコード
ord-502d60fbd0cf4ae9a027c29004ce926b
出典データセット
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07867992B2

反応ノート

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