Sodium Bicarbonate → Ethyl 6,7,8-trifluoro-1-(methylamino)-4-oxo-1,4-dihydroquinoline-3-carboxylate

HRID 1708541ノート

反応式

HRID 1708541 の反応式
Cl.[F:2][C:3]1[CH:4]=[C:5]2[C:10](=[C:11]([F:14])[C:12]=1[F:13])[N:9]([NH:15][CH3:16])[CH:8]=[C:7]([C:17]([O:19][CH2:20][CH3:21])=[O:18])[C:6]2=[O:22].C(=O)([O-])O.[Na+]>ClCCl>[F:2][C:3]1[CH:4]=[C:5]2[C:10](=[C:11]([F:14])[C:12]=1[F:13])[N:9]([NH:15][CH3:16])[CH:8]=[C:7]([C:17]([O:19][CH2:20][CH3:21])=[O:18])[C:6]2=[O:22]

参加物

4

反応物 2

HCID 516892Sodium BicarbonateHCID 67849559HCID 67849559、化合物

生成物 1

HCID 11098599Ethyl 6,7,8-trifluoro-1-(methylamino)-4-oxo-1,4-dihydroquinoline-3-carboxylate収率 97.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of ethyl 6,7,8-trifluoro-1-methylamino-1,4-dihydro -4-oxoquinoline-3-carboxylate hydrochloride(5.91 g)in dichloromethane (100 ml) was added a saturated aqueous sodium hydrogencarbonate solution (50 ml) and the mixture was stirred at ambient temperature for 30 minutes. The organic layer was washed with brine (50 ml), dried over magnesium sulfate, and concentrated under reduced pressure to give a solid. The solid was recrystallized from dichloromethane-n-hexane to give ethyl 6,7,8-trifluoro-1-methylamino-1,4-dihydro-4-oxoquinoline-3-carboxylate (5.14 g).

後処理

  1. washThe organic layer was washed with brine (50 ml)
  2. dry with materialdried over magnesium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customto give a solid
  5. customThe solid was recrystallized from dichloromethane-n-hexane

出典と根拠

ORDレコード
ord-5a48949633a54f27a9bea7505c9f760d
出典データセット
uspto-grants-1994_10
特許番号
US05359066

反応ノート

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