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

HRID 1708541노트

반응식

HRID 1708541 반응식
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]

참가 물질

4

반응물 2

HCID 516892Sodium BicarbonateHCID 67849559HCID 67849559, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-5a48949633a54f27a9bea7505c9f760d
출처 데이터셋
uspto-grants-1994_10
특허 번호
US05359066

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