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Water → Ethyl 1-cyclopropyl-6,7-difluoro-8-methyl-5-nitro-4-oxo-1,4-dihydroquinoline-3-carboxylate

HRID 1078267
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HRID 1078267 반응식
[CH:1]1([NH:4][CH:5]=[C:6]([C:12](=[O:26])[C:13]2[C:18]([N+:19]([O-:21])=[O:20])=[C:17]([F:22])[C:16]([F:23])=[C:15]([CH3:24])[C:14]=2F)[C:7]([O:9][CH2:10][CH3:11])=[O:8])[CH2:3][CH2:2]1.[H-].[Na+].O>O1CCOCC1>[CH:1]1([N:4]2[C:14]3[C:13](=[C:18]([N+:19]([O-:21])=[O:20])[C:17]([F:22])=[C:16]([F:23])[C:15]=3[CH3:24])[C:12](=[O:26])[C:6]([C:7]([O:9][CH2:10][CH3:11])=[O:8])=[CH:5]2)[CH2:3][CH2:2]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 24758Sodium hydrideHCID 178471886HCID 178471886, 화합물

생성물 1

HCID 10736705Ethyl 1-cyclopropyl-6,7-difluoro-8-methyl-5-nitro-4-oxo-1,4-dihydroquinoline-3-carboxylate수율 76%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

To a solution of 27.1 g of ethyl 3-cyclopropylamino-2-(2,4,5-trifluoro-3-methyl-6-nitrobenzoyl)acrylate in 270 ml of 1,4-dioxane, 3.2 g of sodium hydride (60% mineral oil dispersion) was added by portions and stirred at room temperature for one hour. 300 ml of water was added to the reaction mixture and the deposited crystals were collected by filtration to give 19.5 g of the desired compound as colorless crystals, which was recrystallized from N,N-dimethylformamide to provide colorless needles, m.p. 260°-263° C.

후처리

  1. filtrationthe deposited crystals were collected by filtration

출처 및 근거

ORD 기록
ord-9f19ec4c810340dabf3e51866a232595
출처 데이터셋
uspto-grants-1996_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05547962

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