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Water → 3-ethoxycarbonyl-6,7-difluoro-2-[N-cyclopropyl-N-(beta-ethoxycarbonylethyl)amino]quinoline

HRID 375254
노트
인쇄 미리보기

반응식

HRID 375254 반응식
C(=O)([O-])[O-].[Na+].[Na+].Cl[C:8]1[C:17]([C:18]([O:20][CH2:21][CH3:22])=[O:19])=[CH:16][C:15]2[C:10](=[CH:11][C:12]([F:24])=[C:13]([F:23])[CH:14]=2)[N:9]=1.[CH:25]1([NH:28][CH2:29][CH2:30][C:31]([O:33][CH2:34][CH3:35])=[O:32])[CH2:27][CH2:26]1.O>C1(C)C=CC=CC=1.C(O)(=O)C>[CH2:21]([O:20][C:18]([C:17]1[C:8]([N:28]([CH:25]2[CH2:26][CH2:27]2)[CH2:29][CH2:30][C:31]([O:33][CH2:34][CH3:35])=[O:32])=[N:9][C:10]2[C:15]([CH:16]=1)=[CH:14][C:13]([F:23])=[C:12]([F:24])[CH:11]=2)=[O:19])[CH3:22]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 962WaterHCID 10340Sodium CarbonateHCID 97954612-Chloro-3-ethoxycarbonyl-6,7-difluoroquinolineHCID 13456042Ethyl 3-(cyclopropylamino)propanoate

생성물 1

HCID 189945853-ethoxycarbonyl-6,7-difluoro-2-[N-cyclopropyl-N-(beta-ethoxycarbonylethyl)amino]quinoline수율 65.6%

시약·촉매·용매 2

HCID 176
Acetic Acid
용매
HCID 1140Toluene용매

반응 조건

온도
20 °C

실험 절차

3 g of sodium carbonate are added to a solution of 3.48 g of 2-chloro-3-ethoxycarbonyl-6,7-difluoroquinoline and 3 g of N-cyclopropyl-N-(β-ethoxycarbonylethyl)amine in 10 cm3 of toluene. The suspension obtained is heated to reflux and then stirred for 15 hours at this temperature. The reaction mixture is then cooled to approximately 20° C. and 30 cm3 of water and 4.5 cm3 of acetic acid are thereafter added. After settling has taken place, the reaction mixture is separated and washed with twice 10 cm3 of water. The organic phase is concentrated to dryness under reduced pressure (20 kPa) at approximately 50° C. 3.3 g of crude 3-ethoxycarbonyl-6,7-difluoro-2-[N-cyclopropyl-N-(β-ethoxycarbonylethyl)amino]quinoline are obtained in the form of an oil, which is used without further purification for the subsequent step.

후처리

  1. customThe suspension obtained
  2. temperatureis heated
  3. temperatureto reflux
  4. customthe reaction mixture is separated
  5. washwashed with twice 10 cm3 of water
  6. concentrationThe organic phase is concentrated to dryness under reduced pressure (20 kPa) at approximately 50° C

출처 및 근거

ORD 기록
ord-b734297800dd43688690a6e9911a857b
출처 데이터셋
uspto-grants-1996_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05484921

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